ANALYTICAL
CHEMISTRY
Analytical Chemistry
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technologies to support learning.
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for the construction, customization, and dissemination of OER content to reduce the burdens of unreasonable textbook costs to our
students and society. The LibreTexts project is a multi-institutional collaborative venture to develop the next generation of openaccess texts to improve postsecondary education at all levels of higher learning by developing an Open Access Resource
environment. The project currently consists of 14 independently operating and interconnected libraries that are constantly being
optimized by students, faculty, and outside experts to supplant conventional paper-based books. These free textbook alternatives are
organized within a central environment that is both vertically (from advance to basic level) and horizontally (across different fields)
integrated.
The LibreTexts libraries are Powered by NICE CXOne and are supported by the Department of Education Open Textbook Pilot
Project, the UC Davis Office of the Provost, the UC Davis Library, the California State University Affordable Learning Solutions
Program, and Merlot. This material is based upon work supported by the National Science Foundation under Grant No. 1246120,
1525057, and 1413739.
Any opinions, findings, and conclusions or recommendations expressed in this material are those of the author(s) and do not
necessarily reflect the views of the National Science Foundation nor the US Department of Education.
Have questions or comments? For information about adoptions or adaptions contact info@LibreTexts.org. More information on our
activities can be found via Facebook (https://facebook.com/Libretexts), Twitter (https://twitter.com/libretexts), or our blog
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This text was compiled on 01/12/2024
TABLE OF CONTENTS
Licensing
2: Analytical Chemistry 2.0 (Harvey)
00: Front Matter
Table of Contents
1: Front Matter
1.1: TitlePage
1.2: InfoPage
1.3: Table of Contents
2: Introduction to Analytical Chemistry
2.2: The Analytical Perspective
2.3: Common Analytical Problems
2.4: Introduction to Analytical Chemistry (Exercises)
2.5: Introduction to Analytical Chemistry (Summary)
3: Basic Tools of Analytical Chemistry
3.1: Measurements in Analytical Chemistry
3.2: Concentration
3.3: Stoichiometric Calculations
3.4: Basic Equipment
3.5: Preparing Solutions
3.6: Spreadsheets and Computational Software
3.7: The Laboratory Notebook
3.8: Basic Tools of Analytical Chemistry (Exercises)
3.9: Basic Tools of Analytical Chemistry (Summary)
4: The Vocabulary of Analytical Chemistry
4.1: Analysis, Determination, and Measurement
4.2: Techniques, Methods, Procedures, and Protocols
4.3: Classifying Analytical Techniques
4.4: Selecting an Analytical Method
4.5: Developing the Procedure
4.6: Protocols
4.7: The Importance of Analytical Methodology
4.8: The Vocabulary of Analytical Chemistry (Exercises)
4.9: The Vocabulary of Analytical Chemistry (Summary)
5: Evaluating Analytical Data
5.1: Characterizing Measurements and Results
5.2: Characterizing Experimental Errors
5.3: Propagation of Uncertainty
5.4: The Distribution of Measurements and Results
5.5: Statistical Analysis of Data
5.6: Statistical Methods for Normal Distributions
5.7: Detection Limits
5.8: Using Excel and R to Analyze Data
5.9: Evaluating Analytical Data (Exercises)
5.10: Evaluating Analytical Data (Summary)
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6: Standardizing Analytical Methods
6.1: Analytical Standards
6.2: Calibrating the Signal
6.3: Determining the Sensitivity
6.4: Linear Regression and Calibration Curves
6.5: Blank Corrections
6.6: Using Excel and R for a Regression Analysis
6.7: Standardizing Analytical Methods (Exercises)
6.8: Standardizing Analytical Methods (Summary)
7: Equilibrium Chemistry
7.1: Reversible Reactions and Chemical Equilibria
7.2: Thermodynamics and Equilibrium Chemistry
7.3: Manipulating Equilibrium Constants
7.4: Equilibrium Constants for Chemical Reactions
7.5: Le Châtelier’s Principle
7.6: Ladder Diagrams
7.7: Solving Equilibrium Problems
7.8: Buffer Solutions
7.9: Activity Effects
7.10: Using Excel and R to Solve Equilibrium Problems
7.11: Some Final Thoughts on Equilibrium Calculations
7.12: Equilibrium Chemistry (Exercises)
7.13: Equilibrium Chemistry (Summary)
8: Collecting and Preparing Samples
8.1: The Importance of Sampling
8.2: Designing a Sampling Plan
8.3: Implementing the Sampling Plan
8.4: Separating the Analyte from Interferents
8.5: General Theory of Separation Efficiency
8.6: Classifying Separation Techniques
8.7: Liquid–Liquid Extractions
8.8: Separation Versus Preconcentration
8.9: Collecting and Preparing Samples (Exercises)
8.10: Collecting and Preparing Samples (Summary)
9: Gravimetric Methods
9.1: Overview of Gravimetric Methods
9.2: Precipitation Gravimetry
9.3: Volatilization Gravimetry
9.4: Particulate Gravimetry
9.5: Gravimetric Methods (Exercises)
9.6: Gravimetric Methods (Summary)
10: Titrimetric Methods
10.1: Overview of Titrimetry
10.2: Acid–Base Titrations
10.3: Complexation Titrations
10.4: Redox Titrations
10.5: Precipitation Titrations
10.6: Titrimetric Methods (Exercises)
10.7: Titrimetric Methods (Summary)
11: Spectroscopic Methods
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11.1: Overview of Spectroscopy
11.2: Spectroscopy Based on Absorption
11.03: UV
11.3: UV/Vis and IR Spectroscopy
11.4: Atomic Absorption Spectroscopy
11.5: Emission Spectroscopy
11.6: Photoluminescence Spectroscopy
11.7: Atomic Emission Spectroscopy
11.8: Spectroscopy Based on Scattering
11.9: Spectroscopic Methods (Exercises)
11.10: Spectroscopic Methods (Summary)
12: Electrochemical Methods
12.1: Overview of Electrochemistry
12.2: Potentiometric Methods
12.3: Coulometric Methods
12.4: Voltammetric Methods
12.5: Electrochemical Methods (Exercises)
12.6: Electrochemical Methods (Summary)
13: Chromatographic
13.1: Overview of Analytical Separations
13.2: General Theory of Column Chromatography
13.3: Optimizing Chromatographic Separations
13.4: Gas Chromatography
13.5: High-Performance Liquid Chromatography
13.6: Other Forms of Liquid Chromatography
13.7: Electrophoresis
13.8: Chromatographic and Electrophoretic Methods (Exercises)
13.9: Chromatographic and Electrophoretic Methods (Summary)
14: Kinetic Methods
14.1: Kinetic Methods Versus Equilibrium Methods
14.2: Chemical Kinetics
14.3: Radiochemistry
14.4: Flow Injection Analysis
14.5: Kinetic Methods (Exercises)
14.6: Kinetic Methods (Summary)
15: Developing a Standard Method
15.1: Optimizing the Experimental Procedure
15.2: Verifying the Method
15.3: Validating the Method as a Standard Method
15.4: Using Excel and R for an Analysis of Variance
15.5: Developing a Standard Method (Exercises)
15.6: Developing a Standard Method (Summary)
16: Quality Assurance
16.1: The Analytical Perspective—Revisited
16.2: Quality Control
16.3: Quality Assessment
16.4: Evaluating Quality Assurance Data
16.5: Quality Assurance (Exercises)
17: Additional Resources
18: Back Matter
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Index
Glossary
Detailed Licensing
4
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Licensing
A detailed breakdown of this resource's licensing can be found in Back Matter/Detailed Licensing.
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00: Front Matter
This page was auto-generated because a user created a sub-page to this page.
00.1
https://chem.libretexts.org/@go/page/200590
TABLE OF CONTENTS
00: Front Matter
Table of Contents
1: Front Matter
1.1: TitlePage
1.2: InfoPage
1.3: Table of Contents
2: Introduction to Analytical Chemistry
2.2: The Analytical Perspective
2.3: Common Analytical Problems
2.4: Introduction to Analytical Chemistry (Exercises)
2.5: Introduction to Analytical Chemistry (Summary)
3: Basic Tools of Analytical Chemistry
3.1: Measurements in Analytical Chemistry
3.2: Concentration
3.3: Stoichiometric Calculations
3.4: Basic Equipment
3.5: Preparing Solutions
3.6: Spreadsheets and Computational Software
3.7: The Laboratory Notebook
3.8: Basic Tools of Analytical Chemistry (Exercises)
3.9: Basic Tools of Analytical Chemistry (Summary)
4: The Vocabulary of Analytical Chemistry
4.1: Analysis, Determination, and Measurement
4.2: Techniques, Methods, Procedures, and Protocols
4.3: Classifying Analytical Techniques
4.4: Selecting an Analytical Method
4.5: Developing the Procedure
4.6: Protocols
4.7: The Importance of Analytical Methodology
4.8: The Vocabulary of Analytical Chemistry (Exercises)
4.9: The Vocabulary of Analytical Chemistry (Summary)
5: Evaluating Analytical Data
5.1: Characterizing Measurements and Results
5.2: Characterizing Experimental Errors
5.3: Propagation of Uncertainty
5.4: The Distribution of Measurements and Results
5.5: Statistical Analysis of Data
5.6: Statistical Methods for Normal Distributions
5.7: Detection Limits
5.8: Using Excel and R to Analyze Data
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5.9: Evaluating Analytical Data (Exercises)
5.10: Evaluating Analytical Data (Summary)
6: Standardizing Analytical Methods
6.1: Analytical Standards
6.2: Calibrating the Signal
6.3: Determining the Sensitivity
6.4: Linear Regression and Calibration Curves
6.5: Blank Corrections
6.6: Using Excel and R for a Regression Analysis
6.7: Standardizing Analytical Methods (Exercises)
6.8: Standardizing Analytical Methods (Summary)
7: Equilibrium Chemistry
7.1: Reversible Reactions and Chemical Equilibria
7.2: Thermodynamics and Equilibrium Chemistry
7.3: Manipulating Equilibrium Constants
7.4: Equilibrium Constants for Chemical Reactions
7.5: Le Châtelier’s Principle
7.6: Ladder Diagrams
7.7: Solving Equilibrium Problems
7.8: Buffer Solutions
7.9: Activity Effects
7.10: Using Excel and R to Solve Equilibrium Problems
7.11: Some Final Thoughts on Equilibrium Calculations
7.12: Equilibrium Chemistry (Exercises)
7.13: Equilibrium Chemistry (Summary)
8: Collecting and Preparing Samples
8.1: The Importance of Sampling
8.2: Designing a Sampling Plan
8.3: Implementing the Sampling Plan
8.4: Separating the Analyte from Interferents
8.5: General Theory of Separation Efficiency
8.6: Classifying Separation Techniques
8.7: Liquid–Liquid Extractions
8.8: Separation Versus Preconcentration
8.9: Collecting and Preparing Samples (Exercises)
8.10: Collecting and Preparing Samples (Summary)
9: Gravimetric Methods
9.1: Overview of Gravimetric Methods
9.2: Precipitation Gravimetry
9.3: Volatilization Gravimetry
9.4: Particulate Gravimetry
9.5: Gravimetric Methods (Exercises)
9.6: Gravimetric Methods (Summary)
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10: Titrimetric Methods
10.1: Overview of Titrimetry
10.2: Acid–Base Titrations
10.3: Complexation Titrations
10.4: Redox Titrations
10.5: Precipitation Titrations
10.6: Titrimetric Methods (Exercises)
10.7: Titrimetric Methods (Summary)
11: Spectroscopic Methods
11.1: Overview of Spectroscopy
11.2: Spectroscopy Based on Absorption
11.03: UV
11.3: UV/Vis and IR Spectroscopy
11.4: Atomic Absorption Spectroscopy
11.5: Emission Spectroscopy
11.6: Photoluminescence Spectroscopy
11.7: Atomic Emission Spectroscopy
11.8: Spectroscopy Based on Scattering
11.9: Spectroscopic Methods (Exercises)
11.10: Spectroscopic Methods (Summary)
12: Electrochemical Methods
12.1: Overview of Electrochemistry
12.2: Potentiometric Methods
12.3: Coulometric Methods
12.4: Voltammetric Methods
12.5: Electrochemical Methods (Exercises)
12.6: Electrochemical Methods (Summary)
13: Chromatographic
13.1: Overview of Analytical Separations
13.2: General Theory of Column Chromatography
13.3: Optimizing Chromatographic Separations
13.4: Gas Chromatography
13.5: High-Performance Liquid Chromatography
13.6: Other Forms of Liquid Chromatography
13.7: Electrophoresis
13.8: Chromatographic and Electrophoretic Methods (Exercises)
13.9: Chromatographic and Electrophoretic Methods (Summary)
14: Kinetic Methods
14.1: Kinetic Methods Versus Equilibrium Methods
14.2: Chemical Kinetics
14.3: Radiochemistry
14.4: Flow Injection Analysis
14.5: Kinetic Methods (Exercises)
14.6: Kinetic Methods (Summary)
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15: Developing a Standard Method
15.1: Optimizing the Experimental Procedure
15.2: Verifying the Method
15.3: Validating the Method as a Standard Method
15.4: Using Excel and R for an Analysis of Variance
15.5: Developing a Standard Method (Exercises)
15.6: Developing a Standard Method (Summary)
16: Quality Assurance
16.1: The Analytical Perspective—Revisited
16.2: Quality Control
16.3: Quality Assessment
16.4: Evaluating Quality Assurance Data
16.5: Quality Assurance (Exercises)
17: Additional Resources
18: Back Matter
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CHAPTER OVERVIEW
1: Front Matter
1.1: TitlePage
1.2: InfoPage
1.3: Table of Contents
1
DePauw University
Analytical Chemistry 2.1
David Harvey
This text is disseminated via the Open Education Resource (OER) LibreTexts Project (https://LibreTexts.org) and like the hundreds
of other texts available within this powerful platform, it is freely available for reading, printing and "consuming." Most, but not all,
pages in the library have licenses that may allow individuals to make changes, save, and print this book. Carefully
consult the applicable license(s) before pursuing such effects.
Instructors can adopt existing LibreTexts texts or Remix them to quickly build course-specific resources to meet the needs of their
students. Unlike traditional textbooks, LibreTexts’ web based origins allow powerful integration of advanced features and new
technologies to support learning.
The LibreTexts mission is to unite students, faculty and scholars in a cooperative effort to develop an easy-to-use online platform
for the construction, customization, and dissemination of OER content to reduce the burdens of unreasonable textbook costs to our
students and society. The LibreTexts project is a multi-institutional collaborative venture to develop the next generation of openaccess texts to improve postsecondary education at all levels of higher learning by developing an Open Access Resource
environment. The project currently consists of 14 independently operating and interconnected libraries that are constantly being
optimized by students, faculty, and outside experts to supplant conventional paper-based books. These free textbook alternatives are
organized within a central environment that is both vertically (from advance to basic level) and horizontally (across different fields)
integrated.
The LibreTexts libraries are Powered by NICE CXOne and are supported by the Department of Education Open Textbook Pilot
Project, the UC Davis Office of the Provost, the UC Davis Library, the California State University Affordable Learning Solutions
Program, and Merlot. This material is based upon work supported by the National Science Foundation under Grant No. 1246120,
1525057, and 1413739.
Any opinions, findings, and conclusions or recommendations expressed in this material are those of the author(s) and do not
necessarily reflect the views of the National Science Foundation nor the US Department of Education.
Have questions or comments? For information about adoptions or adaptions contact info@LibreTexts.org. More information on our
activities can be found via Facebook (https://facebook.com/Libretexts), Twitter (https://twitter.com/libretexts), or our blog
(http://Blog.Libretexts.org).
This text was compiled on 01/12/2024
1.3: Table of Contents
Analytical chemistry spans nearly all areas of chemistry but involves the development of tools and methods to measure physical
properties of substances and apply those techniques to the identification of their presence (qualitative analysis) and quantify the
amount present (quantitative analysis) of species in a wide variety of settings.
1: Introduction to Analytical Chemistry
1.1: What is Analytical Chemistry?
1.2: The Analytical Perspective
1.3: Common Analytical Problems
1.E: Introduction to Analytical Chemistry (Exercises)
1.S: Introduction to Analytical Chemistry (Summary)
2: Basic Tools of Analytical Chemistry
In the chapters that follow we will explore many aspects of analytical chemistry. In the process we will consider important
questions such as “How do we treat experimental data?”, “How do we ensure that our results are accurate?”, “How do we
obtain a representative sample?”, and “How do we select an appropriate analytical technique?” Before we look more closely at
these and other questions, we will first review some basic tools of importance to analytical chemists.
2.1: Measurements in Analytical Chemistry
2.2: Concentration
2.3: Stoichiometric Calculations
2.4: Basic Equipment
2.5: Preparing Solutions
2.6: Spreadsheets and Computational Software
2.7: The Laboratory Notebook
2.E: Basic Tools of Analytical Chemistry (Exercises)
2.S: Basic Tools of Analytical Chemistry (Summary)
3: The Vocabulary of Analytical Chemistry
If you leaf through an issue of the journal Analytical Chemistry, you will soon discover that the authors and readers share a
common vocabulary of analytical terms. You are probably familiar with some of these terms, such as accuracy and precision,
but other terms, such as analyte and matrix may be less familiar to you. In order to participate in the community of analytical
chemists, you must first understand its vocabulary.
3.1: Analysis, Determination, and Measurement
3.2: Techniques, Methods, Procedures, and Protocols
3.3: Classifying Analytical Techniques
3.4: Selecting an Analytical Method
3.5: Developing the Procedure
3.6: Protocols
3.7: The Importance of Analytical Methodology
3.E: The Vocabulary of Analytical Chemistry (Exercises)
3.S: The Vocabulary of Analytical Chemistry (Summary)
4: Evaluating Analytical Data
When using an analytical method we make three separate evaluations of experimental error. First, before beginning an analysis
we evaluate potential sources of errors to ensure that they will not adversely effect our results. Second, during the analysis we
monitor our measurements to ensure that errors remain acceptable. Finally, at the end of the analysis we evaluate the quality of
the measurements and results, comparing them to our original design criteria.
4.1: Characterizing Measurements and Results
4.2: Characterizing Experimental Errors
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4.3: Propagation of Uncertainty
4.4: The Distribution of Measurements and Results
4.5: Statistical Analysis of Data
4.6: Statistical Methods for Normal Distributions
4.7: Detection Limits
4.8: Using Excel and R to Analyze Data
4.E: Evaluating Analytical Data (Exercises)
4.S: Evaluating Analytical Data (Summary)
5: Standardizing Analytical Methods
Standardization is the process of determining the relationship between the signal and the amount of analyte in a sample.
Previously, we defined this relationship as Stotal=kACA+Sreag where Stotal is the signal, nA is the moles of analyte, CA is the
analyte’s concentration, kA is the method’s sensitivity for the analyte, and Sreag is the contribution to Stotal from sources other
than the sample. To standardize a method we must determine values for kA and Sreag, which is the subject of this chapt
5.1: Analytical Standards
5.2: Calibrating the Signal
5.3: Determining the Sensitivity
5.4: Linear Regression and Calibration Curves
5.5: Blank Corrections
5.6: Using Excel and R for a Regression Analysis
5.E: Standardizing Analytical Methods (Exercises)
5.S: Standardizing Analytical Methods (Summary)
6: Equilibrium Chemistry
Regardless of the problem on which an analytical chemist is working, its solution requires a knowledge of chemistry and the
ability to apply that knowledge. For example, an analytical chemist studying the effect of pollution on spruce trees needs to
know the chemical differences between p‑hydroxybenzoic acid and p‑hydroxyacetophenone, two phenols found in the needles
of spruce trees. Your ability to “think as a chemist” is a product of your experience in the classroom and in the laboratory.
6.1: Reversible Reactions and Chemical Equilibria
6.2: Thermodynamics and Equilibrium Chemistry
6.3: Manipulating Equilibrium Constants
6.4: Equilibrium Constants for Chemical Reactions
6.5: Le Châtelier’s Principle
6.6: Ladder Diagrams
6.7: Solving Equilibrium Problems
6.8: Buffer Solutions
6.9: Activity Effects
6.10: Using Excel and R to Solve Equilibrium Problems
6.11: Some Final Thoughts on Equilibrium Calculations
6.E: Equilibrium Chemistry (Exercises)
6.S: Equilibrium Chemistry (Summary)
7: Collecting and Preparing Samples
When we use an analytical method to solve a problem, there is no guarantee that our results will be accurate or precise. In
designing an analytical method we consider potential sources of determinate error and indeterminate error, and take appropriate
steps to minimize their effect, such as including reagent blanks and calibrating instruments. Why might a carefully designed
analytical method give poor results? One possibility is that we may have failed to account for errors with the sample.
7.1: The Importance of Sampling
7.2: Designing a Sampling Plan
7.3: Implementing the Sampling Plan
7.4: Separating the Analyte from Interferents
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7.5: General Theory of Separation Efficiency
7.6: Classifying Separation Techniques
7.7: Liquid–Liquid Extractions
7.8: Separation Versus Preconcentration
7.E: Collecting and Preparing Samples (Exercises)
7.S: Collecting and Preparing Samples (Summary)
8: Gravimetric Methods
Gravimetry includes all analytical methods in which the analytical signal is a measurement of mass or a change in mass. When
you step on a scale after exercising you are making, in a sense, a gravimetric determination of your mass. Mass is the most
fundamental of all analytical measurements, and gravimetry is unquestionably our oldest quantitative analytical technique.
8.1: Overview of Gravimetric Methods
8.2: Precipitation Gravimetry
8.3: Volatilization Gravimetry
8.4: Particulate Gravimetry
8.E: Gravimetric Methods (Exercises)
8.S: Gravimetric Methods (Summary)
9: Titrimetric Methods
Titrimetry, in which volume serves as the analytical signal, made its first appearance as an analytical method in the early
eighteenth century. Titrimetric methods were not well received by the analytical chemists of that era because they could not
duplicate the accuracy and precision of a gravimetric analysis. Not surprisingly, few standard texts from the 1700s and 1800s
include titrimetric methods of analysis.
9.1: Overview of Titrimetry
9.2: Acid–Base Titrations
9.3: Complexation Titrations
9.4: Redox Titrations
9.5: Precipitation Titrations
9.E: Titrimetric Methods (Exercises)
9.S: Titrimetric Methods (Summary)
10: Spectroscopic Methods
"Colorimetry" is one example of a spectroscopic method of analysis. At the end of the nineteenth century, spectroscopy was
limited to the absorption, emission, and scattering of visible, ultraviolet, and infrared electromagnetic radiation. Since its
introduction, spectroscopy has expanded to include other forms of electromagnetic radiation—such as X-rays, microwaves, and
radio waves—and other energetic particles—such as electrons and ions.
10.1: Overview of Spectroscopy
10.2: Spectroscopy Based on Absorption
10.3: UV/Vis and IR Spectroscopy
10.4: Atomic Absorption Spectroscopy
10.5: Emission Spectroscopy
10.6: Photoluminescence Spectroscopy
10.7: Atomic Emission Spectroscopy
10.8: Spectroscopy Based on Scattering
10.E: Spectroscopic Methods (Exercises)
10.S: Spectroscopic Methods (Summary)
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11: Electrochemical Methods
In Chapter 10 we examined several spectroscopic techniques that take advantage of the interaction between electromagnetic
radiation and matter. In this chapter we turn our attention to electrochemical techniques in which the potential, current, or
charge in an electrochemical cell serves as the analytical signal. Although there are only three basic electrochemical signals,
there are a many possible experimental designs—too many, in fact, to cover adequately in an introductory textbook.
11.1: Overview of Electrochemistry
11.2: Potentiometric Methods
11.3: Coulometric Methods
11.4: Voltammetric Methods
11.E: Electrochemical Methods (Exercises)
11.S: Electrochemical Methods (Summary)
12: Chromatographic & Electrophoretic Methods
For this reason, many analytical procedures include a step to separate the analyte from potential interferents. Although effective,
each additional step in an analytical procedure increases the analysis time and introduces uncertainty. In this chapter we
consider two analytical techniques that avoid these limitations by combining the separation and analysis: chromatography and
electrophoresis.
12.1: Overview of Analytical Separations
12.2: General Theory of Column Chromatography
12.3: Optimizing Chromatographic Separations
12.4: Gas Chromatography
12.5: High-Performance Liquid Chromatography
12.6: Other Forms of Liquid Chromatography
12.7: Electrophoresis
12.E: Chromatographic and Electrophoretic Methods (Exercises)
12.S: Chromatographic and Electrophoretic Methods (Summary)
13: Kinetic Methods
One way to classify analytical techniques is by whether the analyte’s concentration is determined by an equilibrium reaction or
by the kinetics of a chemical reaction or a physical process. Often analytical methods involve measurements made on systems
in which the analyte is always at equilibrium. In this chapter we turn our attention to measurements made under nonequilibrium conditions.
13.1: Kinetic Methods Versus Equilibrium Methods
13.2: Chemical Kinetics
13.3: Radiochemistry
13.4: Flow Injection Analysis
13.E: Kinetic Methods (Exercises)
13.S: Kinetic Methods (Summary)
14: Developing a Standard Method
Among the goals of analytical chemistry are improving established methods of analysis, extending existing methods of analysis
to new types of samples, and developing new analytical methods. In this chapter we discuss how we develop a standard
method, including optimizing the experimental procedure, verifying that the method produces acceptable precision and
accuracy in the hands of a single analyst, and validating the method for general use.
14.1: Optimizing the Experimental Procedure
14.2: Verifying the Method
14.3: Validating the Method as a Standard Method
14.4: Using Excel and R for an Analysis of Variance
14.E: Developing a Standard Method (Exercises)
14.S: Developing a Standard Method (Summary)
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15: Quality Assurance
Knowing that a method meets suitable standards is important if we are to have confidence in our results. Even so, using a
standard method does not guarantee that the result of an analysis is acceptable. In this chapter we introduce the quality
assurance procedures used in industry and government labs for monitoring routine chemical analyses.
15.1: The Analytical Perspective—Revisited
15.2: Quality Control
15.3: Quality Assessment
15.4: Evaluating Quality Assurance Data
15.E: Quality Assurance (Exercises)
Additional Resources
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CHAPTER OVERVIEW
2: Introduction to Analytical Chemistry
Chemistry is the study of matter, including its composition and structure, its physical properties, and its reactivity. There are many
ways to study chemistry, but, we traditionally divide it into five fields: organic chemistry, inorganic chemistry, biochemistry,
physical chemistry, and analytical chemistry. Although this division is historical and, perhaps, arbitrary—as witnessed by current
interest in interdisciplinary areas such as bioanalytical chemistry and organometallic chemistry—these five fields remain the
simplest division spanning the discipline of chemistry.
Topic hierarchy
2.1: What is Analytical Chemistry?
2.2: The Analytical Perspective
2.3: Common Analytical Problems
2.4: Introduction to Analytical Chemistry (Exercises)
2.5: Introduction to Analytical Chemistry (Summary)
Thumbnail: Several graduated cylinders of various thickness and heights with white side markings in front of a large beaker. They
are all filled about halfway with red or blue chemical compounds. The blue ink is showing signs of Brownian motion when
dissolving into water. Image used with permission (CC BY-SA 3.0; Horia Varlan from Bucharest, Romania).
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2.1: What is Analytical Chemistry?
1.1: What is Analytical Chemistry?
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2.2: The Analytical Perspective
1.2: The Analytical Perspective
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2.3: Common Analytical Problems
1.3: Common Analytical Problems
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2.4: Introduction to Analytical Chemistry (Exercises)
1.E: Introduction to Analytical Chemistry (Exercises)
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2.5: Introduction to Analytical Chemistry (Summary)
1.S: Introduction to Analytical Chemistry (Summary)
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CHAPTER OVERVIEW
3: Basic Tools of Analytical Chemistry
In the chapters that follow we will explore many aspects of analytical chemistry. In the process we will consider important
questions such as “How do we treat experimental data?”, “How do we ensure that our results are accurate?”, “How do we obtain a
representative sample?”, and “How do we select an appropriate analytical technique?” Before we look more closely at these and
other questions, we will first review some basic tools of importance to analytical chemists.
3.1: Measurements in Analytical Chemistry
3.2: Concentration
3.3: Stoichiometric Calculations
3.4: Basic Equipment
3.5: Preparing Solutions
3.6: Spreadsheets and Computational Software
3.7: The Laboratory Notebook
3.8: Basic Tools of Analytical Chemistry (Exercises)
3.9: Basic Tools of Analytical Chemistry (Summary)
Thumbnail: A Roberval balance. The pivots of the parallelogram understructure makes it insensitive to load positioning away from
center, so improves its accuracy, and ease of use. Image used with permission (CC BY-SA 3.0; Nikodem Nijaki)
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3.1: Measurements in Analytical Chemistry
2.1: Measurements in Analytical Chemistry
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3.2: Concentration
2.2: Concentration
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3.3: Stoichiometric Calculations
2.3: Stoichiometric Calculations
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3.4: Basic Equipment
2.4: Basic Equipment
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3.5: Preparing Solutions
2.5: Preparing Solutions
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3.6: Spreadsheets and Computational Software
2.6: Spreadsheets and Computational Software
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3.7: The Laboratory Notebook
2.7: The Laboratory Notebook
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3.8: Basic Tools of Analytical Chemistry (Exercises)
2.E: Basic Tools of Analytical Chemistry (Exercises)
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3.9: Basic Tools of Analytical Chemistry (Summary)
2.S: Basic Tools of Analytical Chemistry (Summary)
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CHAPTER OVERVIEW
4: The Vocabulary of Analytical Chemistry
If you leaf through an issue of the journal Analytical Chemistry, you will soon discover that the authors and readers share a
common vocabulary of analytical terms. You are probably familiar with some of these terms, such as accuracy and precision, but
other terms, such as analyte and matrix may be less familiar to you. In order to participate in the community of analytical chemists,
you must first understand its vocabulary. The goal of this chapter, therefore, is to introduce you to some important analytical terms.
Becoming comfortable with these terms will make the material in the chapters that follow easier to read and understand.
4.1: Analysis, Determination, and Measurement
4.2: Techniques, Methods, Procedures, and Protocols
4.3: Classifying Analytical Techniques
4.4: Selecting an Analytical Method
4.5: Developing the Procedure
4.6: Protocols
4.7: The Importance of Analytical Methodology
4.8: The Vocabulary of Analytical Chemistry (Exercises)
4.9: The Vocabulary of Analytical Chemistry (Summary)
Thumbnail: Colonies of fecal coliform bacteria from a water supply. Source: Susan Boyer. Photo courtesy of ARS–USDA
(www.ars.usda.gov). Fecal coliform counts provide a general measure of the presence of pathogenic organisms in a water supply.
For drinking water, the current maximum contaminant level (MCL) for total coliforms, including fecal coliforms is less than 1
colony/100 mL. Municipal water departments must regularly test the water supply and must take action if more than 5% of the
samples in any month test positive for coliform bacteria.
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4.1: Analysis, Determination, and Measurement
3.1: Analysis, Determination, and Measurement
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4.2: Techniques, Methods, Procedures, and Protocols
3.2: Techniques, Methods, Procedures, and Protocols
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4.3: Classifying Analytical Techniques
3.3: Classifying Analytical Techniques
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4.4: Selecting an Analytical Method
3.4: Selecting an Analytical Method
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4.5: Developing the Procedure
3.5: Developing the Procedure
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4.6: Protocols
3.6: Protocols
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4.7: The Importance of Analytical Methodology
3.7: The Importance of Analytical Methodology
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4.8: The Vocabulary of Analytical Chemistry (Exercises)
3.E: The Vocabulary of Analytical Chemistry (Exercises)
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4.9: The Vocabulary of Analytical Chemistry (Summary)
3.S: The Vocabulary of Analytical Chemistry (Summary)
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CHAPTER OVERVIEW
5: Evaluating Analytical Data
When using an analytical method we make three separate evaluations of experimental error. First, before beginning an analysis we
evaluate potential sources of errors to ensure that they will not adversely effect our results. Second, during the analysis we monitor
our measurements to ensure that errors remain acceptable. Finally, at the end of the analysis we evaluate the quality of the
measurements and results, comparing them to our original design criteria. This chapter provides an introduction to sources of error,
to evaluating errors in analytical measurements, and to the statistical analysis of data.
5.1: Characterizing Measurements and Results
5.2: Characterizing Experimental Errors
5.3: Propagation of Uncertainty
5.4: The Distribution of Measurements and Results
5.5: Statistical Analysis of Data
5.6: Statistical Methods for Normal Distributions
5.7: Detection Limits
5.8: Using Excel and R to Analyze Data
5.9: Evaluating Analytical Data (Exercises)
5.10: Evaluating Analytical Data (Summary)
Thumbnail: The blue vertical line segments represent multiple realizations of a confidence interval for the population mean μ,
represented as a red horizontal dashed line; note that some confidence intervals do not contain the population mean, as expected.
Image used with permission (Public Domain; Tsyplakov) .
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5.1: Characterizing Measurements and Results
4.1: Characterizing Measurements and Results
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5.2: Characterizing Experimental Errors
4.2: Characterizing Experimental Errors
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5.3: Propagation of Uncertainty
4.3: Propagation of Uncertainty
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5.4: The Distribution of Measurements and Results
4.4: The Distribution of Measurements and Results
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5.5: Statistical Analysis of Data
4.5: Statistical Analysis of Data
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5.6: Statistical Methods for Normal Distributions
4.6: Statistical Methods for Normal Distributions
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5.7: Detection Limits
4.7: Detection Limits
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5.8: Using Excel and R to Analyze Data
4.8: Using Excel and R to Analyze Data
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5.9: Evaluating Analytical Data (Exercises)
4.E: Evaluating Analytical Data (Exercises)
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5.10: Evaluating Analytical Data (Summary)
4.S: Evaluating Analytical Data (Summary)
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CHAPTER OVERVIEW
6: Standardizing Analytical Methods
The American Chemical Society’s Committee on Environmental Improvement defines standardization as the process of
determining the relationship between the signal and the amount of analyte in a sample.1 In Chapter 3 we defined this relationship as
Stotal = k
A
n
A
+ Sreag
or
Stotal = k
A
C
A
+ Sreag
(6.1)
where S
is the signal, n is the moles of analyte, C is the analyte’s concentration, k is the method’s sensitivity for the
analyte, and S
is the contribution to S
from sources other than the sample. To standardize a method we must determine
values for k and S
. Strategies for accomplishing this are the subject of this chapter.
total
A
reag
A
A
A
total
reag
6.1: Analytical Standards
6.2: Calibrating the Signal
6.3: Determining the Sensitivity
6.4: Linear Regression and Calibration Curves
6.5: Blank Corrections
6.6: Using Excel and R for a Regression Analysis
6.7: Standardizing Analytical Methods (Exercises)
6.8: Standardizing Analytical Methods (Summary)
Thumbnail: Illustration showing the evaluation of a linear regression in which we assume that all uncertainty is the result of
indeterminate errors affecting y. The points in blue, yi, are the original data and the points in red, ŷi, are the predicted values from
the regression equation, ŷ = b0 + b1x. The smaller the total residual error (equation 5.16), the better the fit of the straight-line to
the data
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6.1: Analytical Standards
5.1: Analytical Standards
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6.2: Calibrating the Signal
5.2: Calibrating the Signal
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6.3: Determining the Sensitivity
5.3: Determining the Sensitivity
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6.4: Linear Regression and Calibration Curves
5.4: Linear Regression and Calibration Curves
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6.5: Blank Corrections
5.5: Blank Corrections
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6.6: Using Excel and R for a Regression Analysis
5.6: Using Excel and R for a Regression Analysis
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6.7: Standardizing Analytical Methods (Exercises)
5.E: Standardizing Analytical Methods (Exercises)
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6.8: Standardizing Analytical Methods (Summary)
5.S: Standardizing Analytical Methods (Summary)
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CHAPTER OVERVIEW
7: Equilibrium Chemistry
Regardless of the problem on which an analytical chemist is working, its solution requires a knowledge of chemistry and the ability
to apply that knowledge. For example, an analytical chemist studying the effect of pollution on spruce trees needs to know, or know
where to find, the chemical differences between p‑hydroxybenzoic acid and p‑hydroxyacetophenone, two common phenols found
in the needles of spruce trees. Your ability to “think as a chemist” is a product of your experience in the classroom and in the
laboratory. The material in this text assumes your familiarity with topics from earlier courses. Because of its importance to
analytical chemistry, this chapter provides a review of equilibrium chemistry. Much of the material in this chapter should be
familiar to you, although some topics—ladder diagrams and activity, for example—afford you with new ways to look at
equilibrium chemistry.
7.1: Reversible Reactions and Chemical Equilibria
7.2: Thermodynamics and Equilibrium Chemistry
7.3: Manipulating Equilibrium Constants
7.4: Equilibrium Constants for Chemical Reactions
7.5: Le Châtelier’s Principle
7.6: Ladder Diagrams
7.7: Solving Equilibrium Problems
7.8: Buffer Solutions
7.9: Activity Effects
7.10: Using Excel and R to Solve Equilibrium Problems
7.11: Some Final Thoughts on Equilibrium Calculations
7.12: Equilibrium Chemistry (Exercises)
7.13: Equilibrium Chemistry (Summary)
Thumbnail: The N O ⇌ 2N O
system at Different Temperatures. Nitrogen dioxide (N O ) gas converts to the colorless gas
dinitrogen tetroxide (N O ) at low temperatures, and converts back to N O at higher temperatures. The bottles in this
photograph contain equal amounts of gas at different temperatures. Figure used with permission from Wikipedia (CC BY-SA 3.0).
2
(g)
2
2(g)
2
4
2
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7.1: Reversible Reactions and Chemical Equilibria
6.01: Reversible Reactions and Chemical Equilibria
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7.2: Thermodynamics and Equilibrium Chemistry
6.02: Thermodynamics and Equilibrium Chemistry
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7.3: Manipulating Equilibrium Constants
6.03: Manipulating Equilibrium Constants
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7.4: Equilibrium Constants for Chemical Reactions
6.04: Equilibrium Constants for Chemical Reactions
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7.5: Le Châtelier’s Principle
6.05: Le Châtelier’s Principle
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7.6: Ladder Diagrams
6.06: Ladder Diagrams
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7.7: Solving Equilibrium Problems
6.07: Solving Equilibrium Problems
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7.8: Buffer Solutions
6.08: Buffer Solutions
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7.9: Activity Effects
6.09: Activity Effects
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7.9.1
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7.10: Using Excel and R to Solve Equilibrium Problems
6.10: Using Excel and R to Solve Equilibrium Problems
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7.11: Some Final Thoughts on Equilibrium Calculations
6.11: Some Final Thoughts on Equilibrium Calculations
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7.12: Equilibrium Chemistry (Exercises)
6.E: Equilibrium Chemistry (Exercises)
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7.13: Equilibrium Chemistry (Summary)
6.S: Equilibrium Chemistry (Summary)
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CHAPTER OVERVIEW
8: Collecting and Preparing Samples
When we use an analytical method to solve a problem, there is no guarantee that our results will be accurate or precise. In
designing an analytical method we consider potential sources of determinate error and indeterminate error, and take appropriate
steps to minimize their effect, such as including reagent blanks and calibrating instruments. Why might a carefully designed
analytical method give poor results? One possibility is that we may have failed to account for errors associated with the sample. If
we collect the wrong sample, or if we lose analyte while preparing the sample for analysis, then we introduce a determinate source
of error. If we fail to collect enough samples, or if we collect samples of the wrong size, then our precision may suffer. In this
chapter we consider how collecting samples and preparing them for analysis affects the accuracy and precision of our results.
8.1: The Importance of Sampling
8.2: Designing a Sampling Plan
8.3: Implementing the Sampling Plan
8.4: Separating the Analyte from Interferents
8.5: General Theory of Separation Efficiency
8.6: Classifying Separation Techniques
8.7: Liquid–Liquid Extractions
8.8: Separation Versus Preconcentration
8.9: Collecting and Preparing Samples (Exercises)
8.10: Collecting and Preparing Samples (Summary)
Thumbnail: An example of pipettes and microplates manipulated by an anthropomorphic robot (Andrew Alliance). Image used with
permission (Cc BY-SA 3.0; Pzucchel).
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8.1: The Importance of Sampling
7.1: The Importance of Sampling
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8.2: Designing a Sampling Plan
7.2: Designing a Sampling Plan
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8.3: Implementing the Sampling Plan
7.3: Implementing the Sampling Plan
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8.4: Separating the Analyte from Interferents
7.4: Separating the Analyte from Interferents
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8.5: General Theory of Separation Efficiency
7.5: General Theory of Separation Efficiency
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8.6: Classifying Separation Techniques
7.6: Classifying Separation Techniques
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8.7: Liquid–Liquid Extractions
7.7: Liquid–Liquid Extractions
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8.8: Separation Versus Preconcentration
7.8: Separation Versus Preconcentration
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8.9: Collecting and Preparing Samples (Exercises)
7.E: Collecting and Preparing Samples (Exercises)
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8.10: Collecting and Preparing Samples (Summary)
7.S: Collecting and Preparing Samples (Summary)
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CHAPTER OVERVIEW
9: Gravimetric Methods
Gravimetry includes all analytical methods in which the analytical signal is a measurement of mass or a change in mass. When you
step on a scale after exercising you are making, in a sense, a gravimetric determination of your mass. Mass is the most fundamental
of all analytical measurements, and gravimetry is unquestionably our oldest quantitative analytical technique. The publication in
1540 of Vannoccio Biringuccio’s Pirotechnia is an early example of applying gravimetry—although not yet known by this name—
to the analysis of metals and ores.1 Although gravimetry no longer is the most important analytical method, it continues to find use
in specialized applications.
9.1: Overview of Gravimetric Methods
9.2: Precipitation Gravimetry
9.3: Volatilization Gravimetry
9.4: Particulate Gravimetry
9.5: Gravimetric Methods (Exercises)
9.6: Gravimetric Methods (Summary)
Thumbnails: An analytical balance (Mettler ae-260) that is often used in gravimetric analysis Methods. Image used with
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9.1: Overview of Gravimetric Methods
8.1: Overview of Gravimetric Methods
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9.2: Precipitation Gravimetry
8.2: Precipitation Gravimetry
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9.3: Volatilization Gravimetry
8.3: Volatilization Gravimetry
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9.4: Particulate Gravimetry
8.4: Particulate Gravimetry
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9.5: Gravimetric Methods (Exercises)
8.E: Gravimetric Methods (Exercises)
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9.6: Gravimetric Methods (Summary)
8.S: Gravimetric Methods (Summary)
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CHAPTER OVERVIEW
10: Titrimetric Methods
Titrimetry, in which volume serves as the analytical signal, made its first appearance as an analytical method in the early eighteenth
century. Titrimetric methods were not well received by the analytical chemists of that era because they could not duplicate the
accuracy and precision of a gravimetric analysis. Not surprisingly, few standard texts from the 1700s and 1800s include titrimetric
methods of analysis.
Precipitation gravimetry developed as an analytical method without a general theory of precipitation. An empirical relationship
between a precipitate’s mass and the mass of analyte—what analytical chemists call a gravimetric factor—was determined
experimentally by taking a known mass of analyte through the procedure. Today, we recognize this as an early example of an
external standardization. Gravimetric factors were not calculated using the stoichiometry of a precipitation reaction because
chemical formulas and atomic weights were not yet available! Unlike gravimetry, the development and acceptance of titrimetry
required a deeper understanding of stoichiometry, of thermodynamics, and of chemical equilibria. By the 1900s, the accuracy and
precision of titrimetric methods were comparable to that of gravimetric methods, establishing titrimetry as an accepted analytical
technique.
10.1: Overview of Titrimetry
10.2: Acid–Base Titrations
10.3: Complexation Titrations
10.4: Redox Titrations
10.5: Precipitation Titrations
10.6: Titrimetric Methods (Exercises)
10.7: Titrimetric Methods (Summary)
Thumbnail: A Winkler titration to determine the concentration of dissolved oxygen in a water sample. The dissolved oxygen has
been converted to an equivalent amount of iodine, which is being titrated with thiosulfate using a starch indicator. The blue color in
the flask will disappear when all the iodine has been converted to iodide. Image used with permission (CC BY-SA 3.0; Will
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10.1: Overview of Titrimetry
9.1: Overview of Titrimetry
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10.2: Acid–Base Titrations
9.2: Acid–Base Titrations
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10.3: Complexation Titrations
9.3: Complexation Titrations
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10.4: Redox Titrations
9.4: Redox Titrations
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10.5: Precipitation Titrations
9.5: Precipitation Titrations
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10.6: Titrimetric Methods (Exercises)
9.E: Titrimetric Methods (Exercises)
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10.7: Titrimetric Methods (Summary)
9.S: Titrimetric Methods (Summary)
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CHAPTER OVERVIEW
11: Spectroscopic Methods
An early example of a colorimetric analysis is Nessler’s method for ammonia, which was introduced in 1856. Nessler found that
adding an alkaline solution of HgI2 and KI to a dilute solution of ammonia produces a yellow to reddish brown colloid, with the
colloid’s color depending on the concentration of ammonia. By visually comparing the color of a sample to the colors of a series of
standards, Nessler was able to determine the concentration of ammonia.
Colorimetry, in which a sample absorbs visible light, is one example of a spectroscopic method of analysis. At the end of the
nineteenth century, spectroscopy was limited to the absorption, emission, and scattering of visible, ultraviolet, and infrared
electromagnetic radiation. Since its introduction, spectroscopy has expanded to include other forms of electromagnetic radiation—
such as X-rays, microwaves, and radio waves—and other energetic particles—such as electrons and ions.
11.1: Overview of Spectroscopy
11.2: Spectroscopy Based on Absorption
11.03: UV
11.3: UV/Vis and IR Spectroscopy
11.4: Atomic Absorption Spectroscopy
11.5: Emission Spectroscopy
11.6: Photoluminescence Spectroscopy
11.7: Atomic Emission Spectroscopy
11.8: Spectroscopy Based on Scattering
11.9: Spectroscopic Methods (Exercises)
11.10: Spectroscopic Methods (Summary)
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11.1: Overview of Spectroscopy
10.1: Overview of Spectroscopy
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11.2: Spectroscopy Based on Absorption
10.2: Spectroscopy Based on Absorption
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11.03: UV
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11.3: UV/Vis and IR Spectroscopy
10.3: UV/Vis and IR Spectroscopy
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11.4: Atomic Absorption Spectroscopy
10.4: Atomic Absorption Spectroscopy
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11.5: Emission Spectroscopy
10.5: Emission Spectroscopy
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11.6: Photoluminescence Spectroscopy
10.6: Photoluminescence Spectroscopy
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11.7: Atomic Emission Spectroscopy
10.7: Atomic Emission Spectroscopy
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11.8: Spectroscopy Based on Scattering
10.8: Spectroscopy Based on Scattering
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11.9: Spectroscopic Methods (Exercises)
10.E: Spectroscopic Methods (Exercises)
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11.10: Spectroscopic Methods (Summary)
10.S: Spectroscopic Methods (Summary)
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CHAPTER OVERVIEW
12: Electrochemical Methods
In Chapter 10 we examined several spectroscopic techniques that take advantage of the interaction between electromagnetic
radiation and matter. In this chapter we turn our attention to electrochemical techniques in which the potential, current, or charge in
an electrochemical cell serves as the analytical signal.
Although there are only three basic electrochemical signals, there are a many possible experimental designs—too many, in fact, to
cover adequately in an introductory textbook. The simplest division of electrochemical techniques is between bulk techniques, in
which we measure a property of the solution in the electrochemical cell, and interfacial techniques, in which the potential, charge,
or current depends on the species present at the interface between an electrode and the solution in which it sits. The measurement
of a solution’s conductivity, which is proportional to the total concentration of dissolved ions, is one example of a bulk
electrochemical technique. A determination of pH using a pH electrode is an example of an interfacial electrochemical technique.
Only interfacial electrochemical methods receive further consideration in this chapter.
12.1: Overview of Electrochemistry
12.2: Potentiometric Methods
12.3: Coulometric Methods
12.4: Voltammetric Methods
12.5: Electrochemical Methods (Exercises)
12.6: Electrochemical Methods (Summary)
Thumbnail:Comparison of the current response of a platinum disc electrode in 1 M sulfuric acid given by linear sweep voltammetry
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12.1: Overview of Electrochemistry
11.1: Overview of Electrochemistry
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12.2: Potentiometric Methods
11.2: Potentiometric Methods
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12.3: Coulometric Methods
11.3: Coulometric Methods
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12.4: Voltammetric Methods
11.4: Voltammetric Methods
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12.5: Electrochemical Methods (Exercises)
11.E: Electrochemical Methods (Exercises)
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12.6: Electrochemical Methods (Summary)
11.S: Electrochemical Methods (Summary)
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CHAPTER OVERVIEW
13: Chromatographic
Drawing from an arsenal of analytical techniques—many of which were the subject of the preceding four chapters—analytical
chemists design methods for the analysis of analytes at increasingly lower concentrations and in increasingly more complex
matrices. Despite the power of these analytical techniques, they often suffer from a lack of selectivity. For this reason, many
analytical procedures include a step to separate the analyte from potential interferents. Although effective, each additional step in
an analytical procedure increases the analysis time and introduces uncertainty. In this chapter we consider two analytical techniques
that avoid these limitations by combining the separation and analysis: chromatography and electrophoresis.
13.1: Overview of Analytical Separations
13.2: General Theory of Column Chromatography
13.3: Optimizing Chromatographic Separations
13.4: Gas Chromatography
13.5: High-Performance Liquid Chromatography
13.6: Other Forms of Liquid Chromatography
13.7: Electrophoresis
13.8: Chromatographic and Electrophoretic Methods (Exercises)
13.9: Chromatographic and Electrophoretic Methods (Summary)
Thumbnail: Separation of black ink on a thin layer chromatography plate. Image used with permission (CC BY-SA 3.0; Natrij)}
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13.1: Overview of Analytical Separations
12.1: Overview of Analytical Separations
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13.2: General Theory of Column Chromatography
12.2: General Theory of Column Chromatography
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13.3: Optimizing Chromatographic Separations
12.3: Optimizing Chromatographic Separations
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13.4: Gas Chromatography
12.4: Gas Chromatography
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13.5: High-Performance Liquid Chromatography
12.5: High-Performance Liquid Chromatography
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13.6: Other Forms of Liquid Chromatography
12.6: Other Forms of Liquid Chromatography
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13.7: Electrophoresis
12.7: Electrophoresis
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13.8: Chromatographic and Electrophoretic Methods (Exercises)
12.E: Chromatographic and Electrophoretic Methods (Exercises)
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13.9: Chromatographic and Electrophoretic Methods (Summary)
12.S: Chromatographic and Electrophoretic Methods (Summary)
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CHAPTER OVERVIEW
14: Kinetic Methods
There are many ways to categorize analytical techniques, several of which we introduced in earlier chapters. In Chapter 3 we
classified techniques by whether the signal is proportional to the absolute amount or the relative amount of analyte. For example,
precipitation gravimetry is a total analysis technique because the precipitate’s mass is proportional to the absolute amount, or
moles, of analyte. UV/Vis absorption spectroscopy, on the other hand, is a concentration technique because absorbance is
proportional to the relative amount, or concentration, of analyte.
A second method for classifying analytical techniques is to consider the source of the analytical signal. For example, gravimetry
encompasses all techniques in which the analytical signal is a measurement of mass or a change in mass. Spectroscopy, on the other
hand, includes those techniques in which we probe a sample with an energetic particle, such as the absorption of a photon. This is
the classification scheme used in organizing Chapters 8–11.
Another way to classify analytical techniques is by whether the analyte’s concentration is determined by an equilibrium reaction or
by the kinetics of a chemical reaction or a physical process. The analytical methods described in Chapter 8–11 mostly involve
measurements made on systems in which the analyte is always at equilibrium. In this chapter we turn our attention to
measurements made under non-equilibrium conditions.
14.1: Kinetic Methods Versus Equilibrium Methods
14.2: Chemical Kinetics
14.3: Radiochemistry
14.4: Flow Injection Analysis
14.5: Kinetic Methods (Exercises)
14.6: Kinetic Methods (Summary)
Thumbnail: Determination of a reaction’s intermediate rate from the slope of a line tangent to a curve showing the change in the
analyte’s concentration as a function of time.
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14.1: Kinetic Methods Versus Equilibrium Methods
13.1: Kinetic Methods Versus Equilibrium Methods
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14.2: Chemical Kinetics
13.2: Chemical Kinetics
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14.3: Radiochemistry
13.3: Radiochemistry
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14.4: Flow Injection Analysis
13.4: Flow Injection Analysis
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14.5: Kinetic Methods (Exercises)
13.E: Kinetic Methods (Exercises)
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14.6: Kinetic Methods (Summary)
13.S: Kinetic Methods (Summary)
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CHAPTER OVERVIEW
15: Developing a Standard Method
In Chapter 1 we made a distinction between analytical chemistry and chemical analysis. Among the goals of analytical chemistry
are improving established methods of analysis, extending existing methods of analysis to new types of samples, and developing
new analytical methods. Once we develop a new method, its routine application is best described as chemical analysis. We
recognize the status of these methods by calling them standard methods. Numerous examples of standard methods are presented
and discussed in Chapters 8–13. What we have not yet considered is what constitutes a standard method. In this chapter we discuss
how we develop a standard method, including optimizing the experimental procedure, verifying that the method produces
acceptable precision and accuracy in the hands of a single analyst, and validating the method for general use.
15.1: Optimizing the Experimental Procedure
15.2: Verifying the Method
15.3: Validating the Method as a Standard Method
15.4: Using Excel and R for an Analysis of Variance
15.5: Developing a Standard Method (Exercises)
15.6: Developing a Standard Method (Summary)
Contributors
David Harvey (DePauw University)
This page titled 15: Developing a Standard Method is shared under a CC BY-NC-SA 4.0 license and was authored, remixed, and/or curated by
David Harvey.
1
15.1: Optimizing the Experimental Procedure
14.1: Optimizing the Experimental Procedure
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curated by David Harvey.
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15.2: Verifying the Method
14.2: Verifying the Method
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Harvey.
15.2.1
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15.3: Validating the Method as a Standard Method
14.3: Validating the Method as a Standard Method
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and/or curated by David Harvey.
15.3.1
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15.4: Using Excel and R for an Analysis of Variance
14.4: Using Excel and R for an Analysis of Variance
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and/or curated by David Harvey.
15.4.1
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15.5: Developing a Standard Method (Exercises)
14.E: Developing a Standard Method (Exercises)
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15.6: Developing a Standard Method (Summary)
14.S: Developing a Standard Method (Summary)
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curated by David Harvey.
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CHAPTER OVERVIEW
16: Quality Assurance
In Chapter 14 we discussed the process of developing a standard method, including optimizing the experimental procedure,
verifying that the method produces acceptable precision and accuracy in the hands of a signal analyst, and validating the method
for general use by the broader analytical community. Knowing that a method meets suitable standards is important if we are to have
confidence in our results. Even so, using a standard method does not guarantee that the result of an analysis is acceptable. In this
chapter we introduce the quality assurance procedures used in industry and government labs for monitoring routine chemical
analyses.
16.1: The Analytical Perspective—Revisited
16.2: Quality Control
16.3: Quality Assessment
16.4: Evaluating Quality Assurance Data
16.5: Quality Assurance (Exercises)
Thumbnail: Examples of property control charts that show a sequence of results.
Contributors
David Harvey (DePauw University)
This page titled 16: Quality Assurance is shared under a CC BY-NC-SA 4.0 license and was authored, remixed, and/or curated by David Harvey.
1
16.1: The Analytical Perspective—Revisited
15.1: The Analytical Perspective—Revisited
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curated by David Harvey.
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16.2: Quality Control
15.2: Quality Control
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16.2.1
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16.3: Quality Assessment
15.3: Quality Assessment
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Harvey.
16.3.1
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16.4: Evaluating Quality Assurance Data
15.4: Evaluating Quality Assurance Data
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16.4.1
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16.5: Quality Assurance (Exercises)
15.E: Quality Assurance (Exercises)
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16.5.1
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17: Additional Resources
Gathered here are three types of resources: suggested experiments, mostly from the Journal of Chemical Education and The
Chemical Educator, that provide practical examples of concepts in the textbook; additional readings from the analytical literature
that extend and supplement topics covered in the textbook; and electronic resources, many of which are cataloged in the Analytical
Sciences Digital Library, that help illustrate concepts from the textbook. Although primarily intended for the use of instructors,
these resources also will benefit students who wish to pursue a topic at more depth.
The following experiments provide useful introductions to the statistical analysis of data in the analytical chemistry laboratory.
Bularzik, J. “The Penny Experiment Revisited: An Illustration of Significant Figures, Accuracy, Precision, and Data Analysis,”
J. Chem. Educ. 2007, 84, 1456–1458.
Columbia, M. R. “The Statistics of Coffee: 1. Evaluation of Trace Metals for Establishing a Coffee’s Country of Origin Based
on a Means Comparison,” Chem. Educator 2007, 12, 260–262.
Cunningham, C. C.; Brown, G. R.; St Pierre, L. E. “Evaluation of Experimental Data,” J. Chem. Educ. 1981, 58, 509–511.
Edminston, P. L.; Williams, T. R. “An Analytical Laboratory Experiment in Error Analysis: Repeated Determination of Glucose
Using Commercial Glucometers,” J. Chem. Educ. 2000, 77, 377–379.
Gordus, A. A. “Statistical Evaluation of Class Data for Two Buret Readings,” J. Chem. Educ. 1987, 64, 376–377.
Harvey, D. T. “Statistical Evaluation of Acid/Base Indicators,” J. Chem. Educ. 1991, 68, 329–331.
Hibbert, D. B. “Teaching modern data analysis with The Royal Austrian Chemical Institute’s titration competition,” Aust. J. Ed.
Chem. 2006, 66, 5–11.
Johll, M. E.; Poister, D.; Ferguson, J. “Statistical Comparison of Multiple Methods for the Determination of Dissolved Oxygen
Levels in Natural Water,” Chem. Educator 2002, 7, 146–148.
Jordon, A. D. “Which Method is Most Precise; Which is Most Accurate?,” J. Chem. Educ. 2007, 84, 1459–1460.
Olsen, R. J. “Using Pooled Data and Data Visualization To Introduce Statistical Concepts in the General Chemistry
Laboratory,” J. Chem. Educ. 2008, 85, 544–545.
O’Reilley, J. E. “The Length of a Pestle,” J. Chem. Educ. 1986, 63, 894–896.
Paselk, R. A. “An Experiment for Introducing Statistics to Students of Analytical and Clinical Chemistry,” J. Chem. Educ.
1985, 62, 536.
Puignou, L.; Llauradó, M. “An Experimental Introduction to Interlaboratory Exercises in Analytical Chemistry,” J. Chem.
Educ. 2005, 82, 1079–1081.
Quintar, S. E.; Santagata, J. P.; Villegas, O. I.; Cortinez, V. A. “Detection of Method Effects on Quality of Analytical Data,” J.
Chem. Educ. 2003, 80, 326–329.
Richardson, T. H. “Reproducible Bad Data for Instruction in Statistical Methods,” J. Chem. Educ. 1991, 68, 310–311.
Salzsieder, J. C. “Statistical Analysis Experiment for Freshman Chemistry Lab,” J. Chem. Educ. 1995, 72, 623.
Samide, M. J. “Statistical Comparison of Data in the Analytical Laboratory,” J. Chem. Educ. 2004, 81, 1641–1643.
Sheeran, D. “Copper Content in Synthetic Copper Carbonate: A Statistical Comparison of Experimental and Expected Results,”
J. Chem. Educ. 1998, 75, 453–456.
Spencer, R. D. “The Dependence of Strength in Plastics upon Polymer Chain Length and Chain Orientation,” J. Chem. Educ.
1984, 61, 555–563.
Stolzberg, R. J. “Do New Pennies Lose Their Shells? Hypothesis Testing in the Sophomore Analytical Chemistry Laboratory,”
J. Chem. Educ. 1998, 75, 1453–1455.
Stone, C. A.; Mumaw, L. D. “Practical Experiments in Statistics,” J. Chem. Educ. 1995, 72, 518–524.
Thomasson, K.; Lofthus-Merschman, S.; Humbert, M.; Kulevsky, N. “Applying Statistics in the Undergraduate Chemistry
Laboratory: Experiments with Food Dyes,” J. Chem. Educ. 1998, 75, 231–233.
Vitha, M. F.; Carr, P. W. “A Laboratory Exercise in Statistical Analysis of Data,” J. Chem. Educ. 1997, 74, 998–1000.
A more comprehensive discussion of the analysis of data, covering all topics considered in this chapter as well as additional
material, can be found in any textbook on statistics or data analysis; several such texts are listed here.
Anderson, R. L. Practical Statistics for Analytical Chemists, Van Nostrand Reinhold: New York; 1987.
Graham, R. C. Data Analysis for the Chemical Sciences, VCH Publishers: New York; 1993.
Mark, H.; Workman, J. Statistics in Spectroscopy, Academic Press: Boston; 1991.
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Mason, R. L.; Gunst, R. F.; Hess, J. L. Statistical Design and Analysis of Experiments; Wiley: New York, 1989.
Massart, D. L.; Vandeginste, B. G. M.; Buydens, L. M. C.; De Jong, S.; Lewi, P. J.; Smeyers-Verbeke, J. Handbook of
Chemometrics and Qualimetrics, Elsevier: Amsterdam, 1997.
Miller, J. C.; Miller, J. N. Statistics for Analytical Chemistry, Ellis Horwood PTR Prentice-Hall: New York; 3rd Edition, 1993.
NIST/SEMATECH e-Handbook of Statistical Methods, http://www.itl.nist.gov/div898/handbook/, 2006.
Sharaf, M. H.; Illman, D. L.; Kowalski, B. R. Chemometrics, Wiley-Interscience: New York; 1986.
The importance of defining statistical terms is covered in the following papers.
Analytical Methods Committee “Terminology—the key to understanding analytical science. Part 1: Accuracy, precision and
uncertainty,” AMC Technical Brief No. 13, Sept. 2003 (http://www.rsc.org/lap/rsccom/amc/amc_index.htm).
Goedart, M. J.; Verdonk, A. H. “The Development of Statistical Concepts in a Design-Oriented Laboratory Course in Scientific
Measuring,” J. Chem. Educ. 1991, 68, 1005–1009.
Sánchez, J. M. “Teaching Basic Applied Statistics in University Chemistry Courses: Students’ Misconceptions,” Chem.
Educator 2006, 11, 1–4.
Thompson, M. “Towards a unified model of errors in analytical measurements,” Analyst 2000, 125, 2020–2025.
Treptow, R. S. “Precision and Accuracy in Measurements,” J. Chem. Educ. 1998, 75, 992–995.
The detection of outliers, particularly when working with a small number of samples, is discussed in the following papers.
Analytical Methods Committee “Robust Statistics—How Not To Reject Outliers Part 1. Basic Concepts,” Analyst 1989, 114,
1693–1697.
Analytical Methods Committee “Robust Statistics—How Not to Reject Outliers Part 2. Inter-laboratory Trials,” Analyst 1989,
114, 1699–1702.
Analytical Methods Committee “Robust statistics: a method of coping with outliers,” AMC Technical Brief No. 6, April 2001
(http://www.rsc.org/lap/rsccom/amc/amc_index.htm).
Efstathiou, C. “Stochastic Calculation of Critical Q-Test Values for the Detection of Outliers in Measurements,” J. Chem. Educ.
1992, 69, 773–736.
Efstathiou, C. “Estimation of type 1 error probability from experimental Dixon’s Q parameter on testing for outliers within
small data sets,” Talanta 2006, 69, 1068–1071.
Kelly, P. C. “Outlier Detection in Collaborative Studies,” Anal. Chem. 1990, 73, 58–64.
Mitschele, J. “Small Sample Statistics,” J. Chem. Educ. 1991, 68, 470–473.
The following papers provide additional information on error and uncertainty, including the propagation of uncertainty.
Andraos, J. “On the Propagation of Statistical Errors for a Function of Several Variables,” J. Chem. Educ. 1996, 73, 150–154.
Donato, H.; Metz, C. “A Direct Method for the Propagation of Error Using a Personal Computer Spreadsheet Program,” J.
Chem. Educ. 1988, 65, 867–868.
Gordon, R.; Pickering, M.; Bisson, D. “Uncertainty Analysis by the ‘Worst Case’ Method,” J. Chem. Educ. 1984, 61, 780–781.
Guare, C. J. “Error, Precision and Uncertainty,” J. Chem. Educ. 1991, 68, 649–652.
Guedens, W. J.; Yperman, J.; Mullens, J.; Van Poucke, L. C.; Pauwels, E. J. “Statistical Analysis of Errors: A Practical
Approach for an Undergraduate Chemistry Lab Part 1. The Concept,” J. Chem. Educ. 1993, 70, 776–779
Guedens, W. J.; Yperman, J.; Mullens, J.; Van Poucke, L. C.; Pauwels, E. J. “Statistical Analysis of Errors: A Practical
Approach for an Undergraduate Chemistry Lab Part 2. Some Worked Examples,” J. Chem. Educ. 1993, 70, 838–841.
Heydorn, K. “Detecting Errors in Micro and Trace Analysis by Using Statistics,” Anal. Chim. Acta 1993, 283, 494–499.
Hund, E.; Massart, D. L.; Smeyers-Verbeke, J. “Operational definitions of uncertainty,” Trends Anal. Chem. 2001, 20, 394–406.
Kragten, J. “Calculating Standard Deviations and Confidence Intervals with a Universally Applicable Spreadsheet Technique,”
Analyst 1994, 119, 2161–2165.
Taylor, B. N.; Kuyatt, C. E. “Guidelines for Evaluating and Expressing the Uncertainty of NIST Measurement Results,” NIST
Technical Note 1297, 1994.
Yates, P. C. “A Simple Method for Illustrating Uncertainty Analysis,” J. Chem. Educ. 2001, 78, 770–771.
Consult the following resources for a further discussion of detection limits.
Boumans, P. W. J. M. “Detection Limits and Spectral Interferences in Atomic Emission Spectrometry,” Anal. Chem. 1984, 66,
459A–467A.
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Currie, L. A. “Limits for Qualitative Detection and Quantitative Determination: Application to Radiochemistry,” Anal. Chem.
1968, 40, 586–593.
Currie, L. A. (ed.) Detection in Analytical Chemistry: Importance, Theory and Practice, American Chemical Society:
Washington, D. C., 1988.
Ferrus, R.; Egea, M. R. “Limit of discrimination, limit of detection and sensitivity in analytical systems,” Anal. Chim. Acta
1994, 287, 119–145.
Glaser, J. A.; Foerst, D. L.; McKee, G. D.; Quave, S. A.; Budde, W. L. “Trace analyses for wastewaters,” Environ. Sci. Technol.
1981, 15, 1426–1435.
Kimbrough, D. E.; Wakakuwa, J. “Quality Control Level: An Introduction to Detection Levels,” Environ. Sci. Technol. 1994,
28, 338–345.
The following resources provide additional information on using Excel, including reports of errors in its handling of some
statistical procedures.
McCollough, B. D.; Wilson, B. “On the accuracy of statistical procedures in Microsoft Excel 2000 and Excel XP,” Comput.
Statist. Data Anal. 2002, 40, 713–721.
Morgon, S. L.; Deming, S. N. “Guide to Microsoft Excel for calculations, statistics, and plotting data,”
(http://www.chem.sc.edu/faculty/morgan/resources/Excel/Excel_Guide_Morgan.pdf).
Pottel, H. “Statistical flaws in Excel,” (http://www.coventry.ac.uk/ec/~nhunt/pottel.pdf).
To learn more about using R, consult the following resources.
Chambers, J. M. Software for Data Analysis: Programming with R, Springer: New York, 2008.
Maindonald, J.; Braun, J. Data Analysis and Graphics Using R, Cambridge University Press: Cambridge, UK, 2003.
Sarkar, D. Lattice: Multivariate Data Visualization With R, Springer: New York, 2008.
The following papers provide insight into visualizing data.
Analytical Methods Committee “Representing data distributions with kernel density estimates,” AMC Technical Brief, March
2006 (http://www.rsc.org/lap/rsccom/amc/amc_index.htm).
Frigge, M.; Hoaglin, D. C.; Iglewicz, B. “Some Implementations of the Boxplot,” The American Statistician 1989, 43, 50–54.
Gathered here are links to on-line computational tools, simulations, and tutorials, many of which are found on the Analytical
Sciences Digital Library.
Applets for Statistics (link).
GraphPad QuickCalcs: Free On-Line Calculators (link).
Introduction to Data Analysis (link).
Introduction to Probability and Statistics (link).
Overway, K. “Population versus Sampling Statistics: A Spreadsheet Exercise,” J. Chem. Educ. 2008 85, 749 (link).
Van Bramer, S. E. “A Brief Introduction to the Gaussian Distribution, Sample Statistics, and the Student’s t Statistic,” J. Chem.
Educ. 2007, 84, 1231 (link).
Web Tutorials in Chemistry—Statistics (link).
Chapter 5
Although there are many experiments in the literature that incorporate external standards, the method of standard additions, or
internal standards, the issue of choosing a method standardization is not the experiment’s focus. One experiment designed to
consider the issue of selecting a method of standardization is given here.
Harvey, D. T. “External Standards or Standard Additions? Selecting and Validating a Method of Standardization,” J. Chem.
Educ. 2002, 79, 613–615.
In addition to the texts listed as suggested readings in Chapter 4, the following text provide additional details on linear regression.
Draper, N. R.; Smith, H. Applied Regression Analysis, 2nd. ed.; Wiley: New York, 1981.
The following articles providing more details about linear regression.
Analytical Methods Committee “Is my calibration linear?” AMC Technical Brief, December 2005
(http://www.rsc.org/pdf/amc/brief3.pdf).
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Badertscher, M.; Pretsch, E. “Bad results from good data,” Trends Anal. Chem. 2006, 25, 1131–1138.
Boqué, R.; Rius, F. X.; Massart, D. L. “Straight Line Calibration: Something More Than Slopes, In• tercepts, and Correlation
Coefficients,” J. Chem. Educ. 1993, 70, 230–232.
Danzer, K.; Currie, L. A. “Guidelines for Calibration in Analytical Chemistry. Part 1. Fundamentals and Single Component
Calibration,” Pure Appl. Chem. 1998, 70, 993–1014.
Henderson, G. “Lecture Graphic Aids for Least-Squares Analysis,” J. Chem. Educ. 1988, 65, 1001–1003.
Logan, S. R. “How to Determine the Best Straight Line,” J. Chem. Educ. 1995, 72, 896–898.
Miller, J. N. “Basic Statistical Methods for Analytical Chemistry. Part 2. Calibration and Regression Methods,” Analyst 1991,
116, 3–14.
Renman, L., Jagner, D. “Asymmetric Distribution of Results in Calibration Curve and Standard Addition Evaluations,” Anal.
Chim. Acta 1997, 357, 157–166.
Rodriguez, L. C.; Gamiz-Gracia; Almansa-Lopez, E. M.; Bosque-Sendra, J. M. “Calibration in chemical measurement
processes. II. A methodological approach,” Trends Anal. Chem. 2001, 20, 620–636.
Useful papers providing additional details on the method of standard additions are gathered here.
Bader, M. “A Systematic Approach to Standard Addition Methods in Instrumental Analysis,” J. Chem. Educ. 1980, 57, 703–
706.
Brown, R. J. C.; Roberts, M. R.; Milton, M. J. T. “Systematic error arising form ‘Sequential’ Standard Addition Calibrations. 2.
Determination of Analyte Mass Fraction in Blank Solutions,” Anal. Chim. Acta 2009, 648, 153–156.
Brown, R. J. C.; Roberts, M. R.; Milton, M. J. T. “Systematic error arising form ‘Sequential’ Standard Addition Calibrations:
Quantification and correction,” Anal. Chim. Acta 2007, 587, 158–163.
Bruce, G. R.; Gill, P. S. “Estimates of Precision in a Standard Additions Analysis,” J. Chem. Educ. 1999, 76, 805–807.
Kelly, W. R.; MacDonald, B. S.; Guthrie “Gravimetric Approach to the Standard Addition Method in Instrumental Analysis. 1.”
Anal. Chem. 2008, 80, 6154–6158.
Nimura, Y.; Carr, M. R. “Reduction of the Relative Error in the Standard Additions Method,” Analyst 1990, 115, 1589–1595.
The following papers discusses the importance of weighting experimental data when use linear regression.
Analytical Methods Committee “Why are we weighting?” AMC Technical Brief, June 2007
(http://www.rsc.org/images/brief27_tcm18-92066.pdf)
Karolczak, M. “To Weight or Not to Weight? An Analyst’s Dilemma,” Current Separations 1995, 13, 98–104.
Algorithms for performing a linear regression with errors in both X and Y are discussed in the following papers. Also included here
are papers that address the difficulty of using linear regression to compare two analytical methods.
Irvin, J. A.; Quickenden, T. L. “Linear Least Squares Treatment When There are Errors in Both x and y,” J. Chem. Educ. 1983,
60, 711–712.
Kalantar, A. H. “Kerrich’s Method for y = αx Data When Both y and x Are Uncertain,” J. Chem. Educ. 1991, 68, 368–370.
Macdonald, J. R.; Thompson, W. J. “Least-Squares Fitting When Both Variables Contain Errors: Pitfalls and Possibilities,” Am.
J. Phys. 1992, 60, 66–73.
Martin, R. F. “General Deming Regression for Estimating Systematic Bias and Its Confidence Interval in Method-Comparison
Studies,” Clin. Chem. 2000, 46, 100–104.
Ogren, P. J.; Norton, J. R. “Applying a Simple Linear Least-Squares Algorithm to Data with Uncertainties in Both Variables,” J.
Chem. Educ. 1992, 69, A130–A131.
Ripley, B. D.; Thompson, M. “Regression Techniques for the Detection of Analytical Bias,” Analyst 1987, 112, 377–383.
Outliers present a problem for a linear regression analysis. The following papers discuss the use of robust linear regression
techniques.
Glaister, P. “Robust Linear Regression Using Thiel’s Method,” J. Chem. Educ. 2005, 82, 1472–1473.
Glasser, L. “Dealing with Outliers: Robust, Resistant Regression,” J. Chem. Educ. 2007, 84, 533–534.
Ortiz, M. C.; Sarabia, L. A.; Herrero, A. “Robust regression techniques. A useful alternative for the detection of outlier data in
chemical analysis,” Talanta 2006, 70, 499–512.
The following papers discusses some of the problems with using linear regression to analyze data that has been mathematically
transformed into a linear form, as well as alternative methods of evaluating curvilinear data.
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Chong, D. P. “On the Use of Least Squares to Fit Data in Linear Form,” J. Chem. Educ. 1994, 71, 489–490.
Hinshaw, J. V. “Nonlinear Calibration,” LCGC 2002, 20, 350–355.
Lieb, S. G. “Simplex Method of Nonlinear Least-Squares - A Logical Complementary Method to Linear Least-Squares
Analysis of Data,” J. Chem. Educ. 1997, 74, 1008–1011.
Zielinski, T. J.; Allendoerfer, R. D. “Least Squares Fitting of Nonlinear Data in the Undergraduate Laboratory,” J. Chem. Educ.
1997, 74, 1001–1007.
More information on multivariate and multiple regression can be found in the following papers.
Danzer, K.; Otto, M.; Currie, L. A. “Guidelines for Calibration in Analytical Chemistry. Part 2. Multispecies Calibration,” Pure
Appl. Chem. 2004, 76, 1215–1225.
Escandar, G. M.; Faber, N. M.; Goicoechea, H. C.; de la Pena, A. M.; Olivieri, A.; Poppi, R. J. “Second- and third-order
multivariate calibration: data, algorithms and applications,” Trends Anal. Chem. 2007, 26, 752–765.
Kowalski, B. R.; Seasholtz, M. B. “Recent Developments in Multivariate Calibration,” J. Chemometrics 1991, 5, 129–145.
Lang, P. M.; Kalivas, J. H. “A Global Perspective on Multivariate Calibration Methods,” J. Chemometrics 1993, 7, 153–164.
Madden, S. P.; Wilson, W.; Dong, A.; Geiger, L.; Mecklin, C. J. “Multiple Linear Regression Using a Graphing Calculator,” J.
Chem. Educ. 2004, 81, 903–907.
Olivieri, A. C.; Faber, N. M.; Ferré, J.; Boqué, R.; Kalivas, J. H.; Mark, H. “Uncertainty Estimation and Figures of Merit for
Multivariate Calibration,” Pure Appl. Chem. 2006, 78, 633–661.
An additional discussion on method blanks, including the use of the total Youden blank, is found in the following papers.
Cardone, M. J. “Detection and Determination of Error in Analytical Methodology. Part II. Correction for Corrigible Systematic
Error in the Course of Real Sample Analysis,” J. Assoc. Off. Anal. Chem. 1983, 66, 1283–1294.
Cardone, M. J. “Detection and Determination of Error in Analytical Methodology. Part IIB. Direct Calculational Technique for
Making Corrigible Systematic Error Corrections,” J. Assoc. Off. Anal. Chem. 1985, 68, 199-202.
Ferrus, R.; Torrades, F. “Bias-Free Adjustment of Analytical Methods to Laboratory Samples in Routine Analytical
Procedures,” Anal. Chem. 1988, 60, 1281–1285.
Vitha, M. F.; Carr, P. W.; Mabbott, G. A. “Appropriate Use of Blanks, Standards, and Controls in Chemical Measurements,” J.
Chem. Educ. 2005, 82, 901–902.
There are a variety of computational packages for completing linear regression analyses. These papers provide details on there use
in a variety of contexts.
Espinosa-Mansilla, A.; de la Peña, A. M.; González-Gómez, D. “Using Univariate Linear Regression Calibration Software in
the MATLAB Environment. Application to Chemistry Laboratory Practices,” Chem. Educator 2005, 10, 1–9.
Harris, D. C. “Nonlinear Least-Squares Curve Fitting with Microsoft Excel Solver,” J. Chem. Educ. 1998, 75, 119–121.
Kim, M. S.; Bukart, M.; Kim, M. H. “A Method Visual Interactive Regression,” J. Chem. Educ. 2006, 83, 1884.
Machuca-Herrera, J. G. “Nonlinear Curve Fitting with Spreadsheets,” J. Chem. Educ. 1997, 74, 448–449.
Smith, E. T.; Belogay, E. A.; Hõim “Linear Regression and Error Analysis for Calibration Curves and Standard Additions: An
Excel Spreadsheet Exercise for Undergraduates,” Chem. Educator 2010, 15, 100–102.
Smith, E. T.; Belogay, E. A.; Hõim “Using Multiple Linear Regression to Analyze Mixtures: An Excel Spreadsheet Exercise for
Undergraduates,” Chem. Educator 2010, 15, 103–107.
Young, S. H.; Wierzbicki, A. “Mathcad in the Chemistry Curriculum. Linear Least-Squares Regression,” J. Chem. Educ. 2000,
77, 669.
Young, S. H.; Wierzbicki, A. “Mathcad in the Chemistry Curriculum. Non-Linear Least-Squares Regression,” J. Chem. Educ.
2000, 77, 669.
Gathered here are links to on-line computational tools, simulations, and tutorials, many of which are found on the Analytical
Sciences Digital Library.
Multiple Regression (link).
Non-Parametric Regression with Errors in X and Y (link).
Linear Regression Tutorial (link).
Modeling Data Tutorial (link).
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Chapter 6
The following experiments involve the experimental determination of equilibrium constants, the characterization of buffers, and, in
some cases, demonstrate the importance of activity effects.
“The Effect of Ionic Strength on an Equilibrium Constant (A Class Study)” in Chemical Principles in Practice, J. A. Bell, Ed.,
Addison-Wesley: Reading, MA, 1967.
“Equilibrium Constants for Calcium Iodate Solubility and Iodic Acid Dissociation” in Chemical Principles in Practice, J. A.
Bell, Ed., Addison-Wesley: Reading, MA, 1967.
“The Solubility of Silver Acetate” in Chemical Principles in Practice, J. A. Bell, Ed., Addison-Wesley: Reading, MA, 1967.
Cobb, C. L.; Love, G. A. “Iron(III) Thiocyanate Revisited: A Physical Chemistry Equilibrium Lab Incorporating Ionic Strength
Effects,” J. Chem. Educ. 1998, 75, 90–92.
Green, D. B.; Rechtsteiner, G.; Honodel, A. “Determination of the Thermodynamic Solubility Product, Ksp, of PbI2 Assuming
Nonideal Behavior,” J. Chem. Educ. 1996, 73, 789–792.
Russo, S. O.; Hanania, I. H. “Buffer Capacity,” J. Chem. Educ. 1987, 64, 817–819.
Stolzberg, R. J. “Discovering a Change in Equilibrium Constant with Change in Ionic Strength,” J. Chem. Educ. 1999, 76, 640–
641.
Wiley, J. D. “The Effect of Ionic Strength on the Solubility of an Electrolyte,” J. Chem. Educ. 2004, 81, 1644–1646.
A nice discussion of Berthollet’s discovery of the reversibility of reactions is found in
Roots-Bernstein, R. S. Discovering, Harvard University Press: Cambridge, MA, 1989.
The following texts provide additional coverage of equilibrium chemistry.
Butler, J. N. Ionic Equilibria: A Mathematical Approach; Addison-Wesley: Reading, MA, 1964.
Butler, J. N. Solubility and pH Calculations; Addison-Wesley: Reading, MA, 1973.
Fernando, Q.; Ryan, M. D. Calculations in Analytical Chemistry, Harcourt Brace Jovanovich: New York, 1982.
Freiser, H.; Fernando, Q. Ionic Equilibria in Analytical Chemistry, Wiley: New York, 1963.
Freiser, H. Concepts and Calculations in Analytical Chemistry, CRC Press: Boca Raton, 1992.
Gordus, A. A. Schaum’s Outline of Analytical Chemistry; McGraw-Hill: New York, 1985.
Ramette, R. W. Chemical Equilibrium and Analysis, Addison-Wesley: Reading, MA, 1981.
The following papers discuss a variety of general aspects of equilibrium chemistry.
Gordus, A. A. “Chemical Equilibrium I. The Thermodynamic Equilibrium Concept,” J. Chem. Educ. 1991, 68, 138–140.
Gordus, A. A. “Chemical Equilibrium II. Deriving an Exact Equilibrium Equation,” J. Chem. Educ. 1991, 68, 215–217.
Gordus, A. A. “Chemical Equilibrium III. A Few Math Tricks,” J. Chem. Educ. 1991, 68, 291–293.
Gordus, A. A. “Chemical Equilibrium IV. Weak Acids and Bases,” J. Chem. Educ. 1991, 68, 397–399.
Gordus, A. A. “Chemical Equilibrium VI. Buffer Solutions,” J. Chem. Educ. 1991, 68, 656–658.
Gordus, A. A. “Chemical Equilibrium VII. Precipitates, “J. Chem. Educ. 1991, 68, 927–930.
Thomson, B. M.; Kessick, M. A. “On the Preparation of Buffer Solutions,” J. Chem. Educ. 1981, 58, 743-746.
Weltin, E. “Are the Equilibrium Concentrations for a Chemical Reaction Always Uniquely Determined by the Initial
Concentrations?” J. Chem. Educ. 1990, 67, 548.
Weltin, E. “Are the Equilibrium Compositions Uniquely Determined by the Initial Compositions? Properties of the Gibbs Free
Energy Function,” J. Chem. Educ. 1995, 72, 508–511.
Collected here are a papers discussing a variety of approaches to solving equilibrium problems.
Ault, A. “Do pH in Your Head,” J. Chem. Educ. 1999, 76, 936–938.
Chaston, S. “Calculating Complex Equilibrium Concentrations by a Next Guess Factor Method,” J. Chem. Educ. 1993, 70,
622–624.
Donato, H. “Graphing Calculator Strategies for Solving Chemical Equilibrium Problems,” J. Chem. Educ. 1999, 76, 632–634.
Olivieri, A. C. “Solution of Acid-Base Equilibria by Successive Approximations,” J. Chem. Educ. 1990, 67, 229–231.
Weltin, E. “A Numerical Method to Calculate Equilibrium Concentrations for Single-Equation Systems,” J. Chem. Educ. 1991,
68, 486–487.
Weltin, E. “Calculating Equilibrium Concentrations,” J. Chem. Educ. 1992, 69, 393–396.
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Weltin, E. “Calculating Equilibrium Concentrations for Stepwise Binding of Ligands and Polyprotic Acid-Base Systems,” J.
Chem. Educ. 1993, 70, 568–571.
Weltin, E. “Equilibrium Calculations are Easier Than You Think - But You do Have to Think!” J. Chem. Educ. 1993, 70, 571–
573.
Weltin, E. “Calculating Equilibrium Concentrations by Iteration: Recycle Your Approximations,” J. Chem. Educ. 1995, 72, 36–
38.
Additional historical background on the development of the Henderson-Hasselbalch equation is provided by the following papers.
de Levie, R. “The Henderson Approximation and the Mass Action Law of Guldberg and Waage,” Chem. Educator 2002, 7,
132–135.
de Levie, R. “The Henderson-Hasselbalch Equation: Its History and Limitations,” J. Chem. Educ. 2003, 80, 146.
A simulation is a useful tool for helping students gain an intuitive understanding of a topic. Gathered here are some simulations for
teaching equilibrium chemistry.
Edmonson, L. J.; Lewis, D. L. “Equilibrium Principles: A Game for Students,” J. Chem. Educ. 1999, 76, 502.
Huddle, P. A.; White, M. W.; Rogers, F. “Simulations for Teaching Chemical Equilibrium,” J. Chem. Educ. 2000, 77, 920–926.
The following papers provide additional resources on ionic strength, activity, and the effect of ionic strength and activity on
equilibrium reactions and pH.
Clark, R. W.; Bonicamp, J. M. “The Ksp-Solubility Conundrum,” J. Chem. Educ. 1998, 75, 1182–1185.
de Levie, R. “On Teaching Ionic Activity Effects: What, When, and Where?” J. Chem. Educ. 2005, 82, 878–884.
McCarty, C. G.; Vitz, E. “pH Paradoxes: Demonstrating That It Is Not True That pH = –log[H+],” J. Chem. Educ. 2006, 83,
752–757.
Ramshaw, J. D. “Fugacity and Activity in a Nutshell,” J. Chem. Educ. 1995, 72, 601–603.
Sastre de Vicente, M. E. “The Concept of Ionic Strength Eighty Years After Its Introduction,” J. Chem. Educ. 2004, 81, 750–
753.
Solomon, T. “The Definition and Unit of Ionic Strength,” J. Chem. Educ. 2001, 78, 1691–1692.
For a contrarian’s view of equilibrium chemistry, please see the following papers.
Hawkes, S. J. “Buffer Calculations Deceive and Obscure,” Chem. Educator, 1996, 1, 1–8.
Hawkes, S. J. “What Should We Teach Beginners About Solubility and Solubility Products?” J. Chem. Educ. 1998, 75, 1179–
1181.
Hawkes, S. J. “Complexation Calculations are Worse Than Useless,” J. Chem. Educ. 1999, 76, 1099–1100.
Hawkes, S. J. “Easy Deviation of pH ≈ (pKa1 + pKa2)/2 Using Autoprotolysis of HA–: Doubtful Value of the Supposedly More
Rigorous Equation,” J. Chem. Educ. 2000, 77, 1183–1184. See, also, an exchange of letters between J. J. Roberts and S. J.
Hawkes, J. Chem. Educ. 2002, 79, 161–162.
Chapter 7
The following set of experiments and class exercises introduce students to the importance of sampling on the quality of analytical
results.
Bauer, C. F. “Sampling Error Lecture Demonstration,” J. Chem. Educ. 1985, 62, 253.
Canaes, L. S.; Brancalion, M. L.; Rossi, A. V.; Rath, S. “Using Candy Samples to Learn About Sampling Techniques and
Statistical Evaluation of Data,” J. Chem. Educ. 2008, 85, 1083–1088.
Clement, R. E. “Environmental Sampling for Trace Analysis,” Anal. Chem. 1992, 64, 1076A–1081A.
Dunn, J. G.; Phillips, D. N.; van Bronswijk, W. “An Exercise to Illustrate the Importance of Sample Preparation in Chemical
Analysis,” J. Chem. Educ. 1997, 74, 1188–1191.
Fritz, M. D. “A Demonstration of Sample Segregation,” J. Chem. Educ. 2005, 82, 255–256.
Guy, R. D.; Ramaley, L.; Wentzell, P. D. “An Experiment in the Sampling of Solids for Chemical Analysis”, J. Chem. Educ.
1998, 75, 1028-1033.
Hartman, J. R. “An In-Class Experiment to Illustrate the Importance of Sampling Techniques and Statistical Analysis of Data to
Quantitative Analysis Students,” J. Chem. Educ. 2000, 77, 1017–1018.
Harvey, D. T. “Two Experiments Illustrating the Importance of Sampling in a Quantitative Chemical Analysis,” J. Chem. Educ.
2002, 79, 360–363.
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Herrington, B. L. “A Demonstration of the Necessity for Care in Sampling,” J. Chem. Educ. 1937, 14, 544.
Kratochvil, B.; Reid, R. S.; Harris, W. E. “Sampling Error in a Particulate Mixture”, J. Chem. Educ. 1980, 57, 518–520.
Ross, M. R. “A Classroom Exercise in Sampling Technique,” J. Chem. Educ. 2000, 77, 1015–1016.
Settle, F. A.; Pleva, M. “The Weakest Link Exercise,” Anal. Chem. 1999, 71, 538A–540A.
Vitt, J. E.; Engstrom, R. C. “Effect of Sample Size on Sampling Error,” J. Chem. Educ. 1999, 76, 99–100.
The following experiments describe homemade sampling devices for collecting samples in the field.
Delumyea, R. D.; McCleary, D. L. “A Device to Collect Sediment Cores,” J. Chem. Educ. 1993, 70, 172–173.
Rockwell, D. M.; Hansen, T. “Sampling and Analyzing Air Pollution,” J. Chem. Educ. 1994, 71, 318–322.
Saxena, S., Upadhyay, R.; Upadhyay, P. “A Simple and Low-Cost Air Sampler,” J. Chem. Educ. 1996, 73, 787–788.
Shooter, D. “Nitrogen Dioxide and Its Determination in the Atmosphere,” J. Chem. Educ. 1993, 70, A133–A140.
The following experiments introduce students to methods for extracting analytes from their matrix.
“Extract-Clean™ SPE Sample Preparation Guide Volume 1”, Bulletin No. 83, Alltech Associates, Inc. Deerfield, IL.
Freeman, R. G.; McCurdy, D. L. “Using Microwave Sample Decomposition in Undergraduate Analytical Chemistry,” J. Chem.
Educ. 1998, 75, 1033–1032.
Snow, N. H.; Dunn, M.; Patel, S. “Determination of Crude Fat in Food Products by Supercritical Fluid Extraction and
Gravimetric Analysis,” J. Chem. Educ. 1997, 74, 1108–1111.
Yang, M. J.; Orton, M. L.; Pawliszyn, J. “Quantitative Determination of Caffeine in Beverages Using a Combined SPMEGC/MS Method,” J. Chem. Educ. 1997, 74, 1130–1132.
The following paper provides a general introduction to the terminology used in describing sampling.
“Terminology—The key to understanding analytical science. Part 2: Sampling and sample preparation,” AMC Technical Brief
No. 19, March 2005 (link).
Majors, R. E. “Nomenclature for Sampling in Analytical Chemistry” LC•GC 1992, 10, 500–506.
Further information on the statistics of sampling is covered in the following papers and textbooks.
“What is uncertainty from sampling, and why is it important?” AMC Technical Brief No. 16A, June 2004 (link).
“Analytical and sampling strategy, fitness for purpose, and computer games,” AMC Technical Brief No. 20, August 2005 (link).
“Measurement uncertainty arising from sampling: the new Eurachem Guide,” AMC Technical Brief No. 31, July 2008 (link).
Sampling for Analytical Purpose, Gy, P. ed., Wiley: NY, 1998.
Baiulescu, G. E.; Dumitrescu, P.; Zuaravescu, P. G. Sampling, Ellis Horwood: NY, 1991.
Cohen, R. D. “How the Size of a Random Sample Affects How Accurately It Represents a Population,” J. Chem. Educ. 1992,
74, 1130–1132.
Efstathiou, C. E. “On the sampling variance of ultra-dilute solutions,” Talanta 2000, 52, 711–715.
Gerlach, R. W.; Dobb, D. E.; Raab, G. A.; Nocerino, J. M. J. Chemom. 2002, 16, 321–328.
Gy, P. M. Sampling of Particulate Materials: Theory and Practice; Elsevier: Amsterdam, 1979.
Gy, P. M. Sampling of Heterogeneous and Dynamic Materials: Theories of Heterogeneity, Sampling and Homogenizing;
Elsevier: Amsterdam, 1992.
Kratochvil, B.; Taylor, J. K. “Sampling for Chemical Analysis,” Anal. Chem. 1981, 53, 924A–938A.
Kratochvil, B.; Goewie, C. E.; Taylor, J. K. “Sampling Theory for Environmental Analysis,” Trends Anal. Chem. 1986, 5, 253–
256.
Meyer, V. R. LC•GC 2002, 20, 106–112.
Rohlf, F. J.; Akçakaya, H. R.; Ferraro, S. P. “Optimizing Composite Sampling Protocols,” Environ. Sci. Technol. 1996, 30,
2899–2905.
Smith, R.; James, G. V. The Sampling of Bulk Materials; Royal Society of Chemistry: London, 1981.
The process of collecting a sample presents a variety of difficulties, particularly with respect to the analyte’s integrity. The
following papers provide representative examples of sampling problems.
Barceló, D.; Hennion, M. C. “Sampling of Polar Pesticides from Water Matrices,” Anal. Chim. Acta 1997, 338, 3–18.
Batley, G. E.; Gardner, D. “Sampling and Storage of Natural Waters for Trace Metal Analysis,” Wat. Res. 1977, 11, 745–756.
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Benoit, G.; Hunter, K. S.; Rozan, T. F. “Sources of Trace Metal Contamination Artifacts during Collection, Handling, and
Analysis of Freshwaters,” Anal. Chem. 1997, 69, 1006–1011
Brittain, H. G. “Particle-Size Distribution II: The Problem of Sampling Powdered Solids,” Pharm. Technol. July 2002, 67–73.
Ramsey, M. H. “Measurement Uncertainty Arising from Sampling: Implications for the Objectives of Geoanalysis,” Analyst,
1997, 122, 1255–1260.
Seiler, T-B; Schulze, T.; Hollert, H. “The risk of altering soil and sediment samples upon extract preparation for analytical and
bio-analytical investigations—a review,” Anal. Bioanal. Chem. 2008, 390, 1975–1985.
The following texts and articles provide additional information on methods for separating analytes and interferents.
“Guide to Solid Phase Extraction,” Bulletin 910, Sigma-Aldrich, 1998.
“Solid Phase Microextraction: Theory and Optimization of Conditions,” Bulletin 923, Sigma-Aldrich, 1998.
Microwave-Enhanced Chemistry: Fundamentals, Sample Preparation, and Applications, Kingston, H. M.; Haswell, S. J., eds.;
American Chemical Society: Washington, D.C., 1997.
Anderson, R. Sample Pretreatment and Separation, Wiley: Chichester, 1987.
Bettiol, C.; Stievano, L.; Bertelle, M.; Delfino, F.; Argese, E. “Evaluation of microwave-assisted acid extraction procedures for
the determination of metal content and potential bioavailability in sediments,” Appl. Geochem. 2008, 23, 1140–1151.
Compton, T. R. Direct Preconcentration Techniques, Oxford Science Publications: Oxford, 1993.
Compton, T. R. Complex-Formation Preconcentration Techniques, Oxford Science Publications: Oxford, 1993.
Hinshaw, J. V. “Solid-Phase Microextraction,” LC•GC Europse 2003, December, 2–5.
Karger, B. L.; Snyder, L. R.; Harvath, C. An Introduction to Separation Science, Wiley-Interscience: N. Y.; 1973.
Majors, R. E.; Raynie, D. E. “Sample Preparation and Solid-Phase Extraction”, LC•GC 1997, 15, 1106–1117.
Luque de Castro, M. D.; Priego-Capote, F.; Sánchez-Ávila, N. “Is dialysis alive as a membrane-based separation technique?”
Trends Anal. Chem. 2008, 27, 315–326.
Mary, P.; Studer, V.; Tabeling, P. “Microfluidic Droplet-Based Liquid–Liquid Extraction,” Anal. Chem. 2008, 80, 2680–2687.
Miller, J. M. Separation Methods in Chemical Analysis, Wiley-Interscience: N. Y.; 1975.
Morrison, G. H.; Freiser, H. Solvent Extraction in Analytical Chemistry, John Wiley and Sons: N. Y.; 1957.
Pawliszyn, J. Solid-Phase Microextraction: Theory and Practice, Wiley: NY, 1997.
Pawliszyn, J. “Sample Preparation: Quo Vadis?” Anal. Chem. 2003, 75, 2543–2558.
Sulcek, Z.; Povondra, P. Methods of Decomposition in Inorganic Analysis; CRC Press: Boca Raton, FL, 1989.
Theis, A. L.; Waldack, A. J.; Hansen, S. M.; Jeannot, M. A. “Headspace Solvent Microextraction,” Anal. Chem. 2001, 73,
5651–5654.
Thurman, E. M.; Mills, M. S. Solid-Phase Extraction: Principles and Practice, Wiley: NY, 1998.
Zhang, Z.; Yang, M.; Pawliszyn, J. “Solid-Phase Microextraction,” Anal. Chem. 1994, 66, 844A–853A.
Chapter 8
The following set of experiments introduce students to the applications of gravimetry.
Burrows, H. D.; Ellis, H. A.; Odilora, C. A. “The Dehydrochlorination of PVC,” J. Chem. Educ. 1995, 72, 448–450.
Carmosini, N.; Ghoreshy, S. Koether, M. C. “The Gravimetric Analysis of Nickel Using a Microwave Oven,” J. Chem. Educ.
1997, 74, 986–987.
Harris, T. M. “Revitalizing the Gravimetric Determination in Quantitative Analysis Laboratory,” J. Chem. Educ. 1995, 72, 355–
356.
Henrickson, C. H.; Robinson, P. R. “Gravimetric Determination of Calcium as CaC2O4•H2O,” J. Chem. Educ. 1979, 56, 341–
342.
Shaver, L. A. “Determination of Phosphates by the Gravimetric Quimociac Technique,” J. Chem. Educ. 2008, 85, 1097–1098.
Snow, N. H.; Dunn, M.; Patel, S. “Determination of Crude Fat in Food Products by Supercritical Fluid Extraction and
Gravimetric Analysis,” J. Chem. Educ. 1997, 74, 1108–1111.
Thompson, R. Q.; Ghadiali, M. “Microwave Drying of Precipitates for Gravimetric Analysis,” J. Chem. Educ. 1993, 70, 170–
171.
Wynne, A. M. “The Thermal Decomposition of Urea,” J. Chem. Educ. 1987, 64, 180–182.
The following resources provide a general history of gravimetry.
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A History of Analytical Chemistry; Laitinen, H. A.; Ewing, G. W., Eds.; The Division of Analytical Chemistry of the American
Chemical Society: Washington, D. C., 1977, pp. 10-24.
Beck, C. M. “Classical Analysis: A Look at the Past, Present, and Future,” Anal. Chem. 1991, 63, 993A–1003A; Anal. Chem.
1994, 66, 224A–239A
Consult the following texts for additional examples of inorganic and organic gravimetric methods include the following texts.
Bassett, J.; Denney, R. C.; Jeffery, G. H.; Mendham, J. Vogel’s Textbook of Quantitative Inorganic Analysis, Longman: London,
4th Ed., 1981.
Erdey, L. Gravimetric Analysis, Pergamon: Oxford, 1965.
Steymark, A. Quantitative Organic Microanalysis, The Blakiston Co.: NY, 1951.
Wendlandt, W. W. Thermal Methods of Analysis, 2nd Ed. Wiley: NY. 1986.
For a review of isotope dilution mass spectrometry see the following article.
Fassett, J. D.; Paulsen, P. J. “Isotope Dilution Mass Spectrometry for Accurate Elemental Analysis,” Anal. Chem. 1989, 61,
643A–649A.
Chapter 9
The following set of experiments introduce students to the applications of titrimetry. Experiments are grouped into four categories
based on the type of reaction (acid–base, complexation, redox, and precipitation). Additional experiments emphasizing
potentiometric electrodes are found in Chapter 11.
Acid–base titrimetry
Boiani, J. A. “The Gran Plot Analysis of an Acid Mixture,” J. Chem. Educ. 1986, 63, 724–726.
Castillo, C. A.; Jaramillo, A. “An Alternative Procedure for Titration Curves of a Mixture of Acids of Different Strengths,” J.
Chem. Educ. 1989, 66, 341.
Clark, R. W.; White, G. D.; Bonicamp, J. M.; Watts, E. D. “From Titration Data to Buffer Capacities: A Compter Experiment
for the Chemistry Lab or Lecture,” J. Chem. Educ. 1995, 72, 746–750.
Clay, J. T.; Walters, E. A.; Brabson, G. D. “A Dibasic Acid Titration for the Physical Chemistry Laboratory” J. Chem. Educ.
1995, 72, 665–667.
Crossno, S. K; Kalbus, L. H.; Kalbus, G. E. “Determinations of Carbon Dioxide by Titration,” J. Chem. Educ. 1996, 73, 175–
176.
Flowers, P. A. “Potentiometric Measurement of Transition Ranges and Titration Errors for Acid/Base Indicators,” J. Chem.
Educ. 1997, 74, 846–847.
Fuchsam, W. H.; Garg, Sandhya “Acid Content of Beverages,” J. Chem. Educ. 1990, 67, 67–68
Graham. R.C.; DePew, S. “Determination of Ammonia in Household Cleaners,” J. Chem. Educ. 1983, 60, 765–766.
Kalbus, L. H.; Petrucci, R. H.; Forman, J. E.; Kalbus, G. E. “Titration of Chromate-Dichromate Mixtures,” J. Chem. Educ.
1991, 68, 677–678.
Kooser, A. S.; Jenkins, J. L.; Welch, L. E. “Acid–Base Indicators: A New Look at an Old Topic,” J. Chem. Educ. 2001, 78,
1504–1506.
Kraft, A. “The Determination of the pKa of Multiprotic, Weak Acids by Analyzing Potentiometric Acid–Base Titration Data
with Difference Plots,” J. Chem. Educ. 2003, 80, 554–559.
Murphy, J. “Determination of Phosphoric Acid in Cola Beverages,” J. Chem. Educ. 1983, 60, 420–421.
Nyasulu, F.; Barlag, R.; Macklin, J. Chem. Educator 2008, 13, 289–294.
Ophardt, C. E. “Acid Rain Analysis by Standard Addition Titration,” J. Chem. Educ. 1985, 62, 257–258.
Partanen, J. I.; Kärki, M. H. “Determination of the Thermodynamic Dissociation Constant of a Weak Acid by Potentiometric
Acid-Base Titration,” J. Chem. Educ. 1994, 71, A120–A122.
Thompson, R. Q. “Identification of Weak Acids and Bases by Titration with Primary Standards,” J. Chem. Educ. 1988, 65,
179–180.
Tucker, S. A.; Amszi, V. L.; Acree, Jr. W. E. “Studying Acid-Base Equilibria in Two-Phase Solvent Media,” J. Chem. Educ.
1993, 70, 80–82.
Tucker, S. A.; Acree, Jr., W. E. “A Student-Designed Analytical Laboratory Method,” J. Chem. Educ. 1994, 71, 71–74.
Werner, J. A.; Werner, T. C. “Multifunctional Base Unknowns in the Introductory Analytical Chemistry Lab,” J. Chem. Educ.
1991, 68, 600–601.
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Complexation Titrimetry
Ceretti, H.; Hughes, E. A.; Zalts, A. “The Softening of Hard Water and Complexometric Titrations,” J. Chem. Educ. 1999, 76,
1420–1421.
Fulton, R.; Ross, M.; Schroeder, K. “Spectrophotometric Titration of a Mixture of Calcium and Magnesium,” J. Chem. Educ.
1986, 63, 721–723.
Novick, S. G. “Complexometric Titration of Zinc,” J. Chem. Educ. 1997, 74, 1463.
Olsen, K. G.; Ulicny, L. J. “Reduction of Calcium Concentrations by the Brita Water Filtration System: A Practical Experiment
in Titrimetry and Atomic Absorption Spectroscopy,” J. Chem. Educ. 2001, 78, 941.
Smith, R. L.; Popham, R. E. “The Quantitative Resolution of a Mixture of Group II Metal Ions by Thermometric Titration with
EDTA,” J. Chem. Educ. 1983, 60, 1076–1077.
Yappert, M. C.; DuPré, D. B. “Complexometric Titrations: Competition of Complexing Agents in the Determination of Water
Hardness with EDTA,” J. Chem. Educ. 1997, 74, 1422–1423.
Redox Titrimetry
Guenther, W. B. “Supertitrations: High-Precision Methods,” J. Chem. Educ. 1988, 65, 1097–1098.
Haddad, P. “Vitamin C Content of Commercial Orange Juices,” J. Chem. Educ. 1977, 54, 192–193.
Harris, D. C.; Hills, M. E.; Hewston, T. A. “Preparation, Iodometric Analysis and Classroom Demonstration of
Superconductivity in YBa2Cu3O8–x,” J. Chem. Educ. 1987, 64, 847–850.
Lau, O.-W.; Luk, S.-F.; Cheng, N. L. N.; Woo, H.-O. “Determination of Free Lime in Clinker and Cement by Iodometry,” J.
Chem. Educ. 2001, 78, 1671–1673.
Phinyocheep, P.; Tang, I. M. “Determination of the Hole Concentration (Copper Valency) in the High Tc Superconductors,” J.
Chem. Educ. 1994, 71, A115–A118.
Powell, J. R.; Tucker, S. A.; Acree, Jr., W. E.; Sees, J. A.; Hall, L. M. “A Student-Designed Potentiometric Titration:
Quantitative Determination of Iron(II) by Caro’s Acid Titration,” J. Chem. Educ. 1996, 73, 984–986.
Precipitation Titrimetry
Ueno, K.; Kina, K. “Colloid Titration - A Rapid Method for the Determination of Charged Colloid,” J. Chem. Educ. 1985, 62,
627–629.
For a general history of titrimetry, see the following sources.
A History of Analytical Chemistry; Laitinen, H. A.; Ewing, G. W., Eds.; The Division of Analytical Chemistry of the American
Chemical Society: Washington, D. C., 1977, pp. 52–93.
Kolthoff, I. M. “Analytical Chemistry in the USA in the First Quarter of This Century,” Anal. Chem. 1994, 66, 241A–249A.
The use of weight instead of volume as a signal for titrimetry is reviewed in the following paper.
Kratochvil, B.; Maitra, C. “Weight Titrations: Past and Present,” Am. Lab. 1983, January, 22–29.
A more thorough discussion of non-aqueous titrations, with numerous practical examples, is provided in the following text.
Fritz, J. S. Acid-Base Titrations in Nonaqueous Solvents; Allyn and Bacon, Boston; 1973.
The sources listed below provides more details on the how potentiometric titration data may be used to calculate equilibrium
constants.
Babić, S.; Horvat, A. J. M.; Pavlović, D. M.; Kaštelan-Macan, M. “Determination of pKa values of active pharmaceutical
ingredients,” Trends Anal. Chem. 2007, 26, 1043–1061.
Meloun, M.; Havel, J.; Högfeldt, E. Computation of Solution Equilibria, Ellis Horwood Limited: Chichester, England; 1988.
The following provides additional information about Gran plots.
Michalowski, T.; Kupiec, K.; Rymanowski, M. Anal. Chim. Acta 2008, 606, 172–183.
Schwartz, L. M. “Advances in Acid-Base Gran Plot Methodology,” J. Chem. Educ. 1987, 64, 947–950.
Schwartz, L. M. “Uncertainty of a Titration Equivalence Point,” J. Chem. Educ. 1992, 69, 879–883.
The following provide additional information about calculating or sketching titration curves.
Barnum, D. “Predicting Acid–Base Titration Curves without Calculations,” J. Chem. Educ. 1999, 76, 938–942.
de Levie, R. “A simple expression for the redox titration curve,” J. Electroanal. Chem. 1992, 323, 347–355.
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King, D. W. “A General Approach for Calculating Speciation and Posing Capacity of Redox Systems with Multiple Oxidation
States: Application to Redox Titrations and the Generation of pε–pH,” J. Chem. Educ. 2002, 79, 1135–1140.
For a complete discussion of the application of complexation titrimetry see the texts listed below.
Pribil, R. Applied Complexometry, Pergamon Press: Oxford, 1982.
Ringbom, A. Complexation in Analytical Chemistry, John Wiley and Sons, Inc.: New York, 1963.
Schwarzenbach, G. Complexometric Titrations, Methuen & Co. Ltd: London, 1957.
A good source for additional examples of the application of all forms of titrimetry is
Vogel’s Textbook of Quantitative Inorganic Analysis, Longman: London, 4th Ed., 1981.
Chapter 10
The following set of experiments introduce students to the applications of spectroscopy. Experiments are grouped into five
categories: UV/Vis spectroscopy, IR spectroscopy, atomic absorption and atomic emission, fluorescence and phosphorescence, and
signal averaging.
UV/Vis Spectroscopy
Abney, J. R.; Scalettar, B. A. “Saving Your Students’ Skin. Undergraduate Experiments That Probe UV Protection by
Sunscreens and Sunglasses,” J. Chem. Educ. 1998, 75, 757–760.
Ainscough, E. W.; Brodie, A. M. “The Determination of Vanillin in Vanilla Extract,” J. Chem. Educ. 1990, 67, 1070–1071.
Allen, H. C.; Brauers, T.; Finlayson-Pitts, B. J. “Illustrating Deviations in the Beer-Lambert Law in an Instrumental Analysis
Laboratory: Measuring Atmospheric Pollutants by Differential Optical Absorption Spectrometry,” J. Chem. Educ. 1997, 74,
1459–1462.
Blanco, M.; Iturriaga, H.; Maspoch, S.; Tarîn, P. “A Simple Method for Spectrophotometric Determination of Two-Components
with Overlapped Spectra,” J. Chem. Educ. 1989, 66, 178–180.
Bonicamp, J. M.; Martin, K. L.; McBride, G. R.; Clark, R. W. “Beer’s Law is Not a Straight Line: Amplification of Errors by
Transformation,” Chem. Educator 1999, 4, 81–88.
Bruneau, E.; Lavabre, D.; Levy, G.; Micheau, J. C. “Quantitative Analysis of Continuous-Variation Plots with a Comparison of
Several Methods,” J. Chem. Educ. 1992, 69, 833–837.
Cappas, C.; Hoffman, N.; Jones, J.; Young, S. “Determination of Concentrations of Species Whose Absorption Bands Overlap
Extensively,” J. Chem. Educ. 1991, 68, 300–303.
Crisp, P. T.; Eckert, J. M.; Gibson, N. A. “The Determination of Anionic Surfactants in Natural and Waste Waters,” J. Chem.
Educ. 1983, 60, 236–238.
Dilbeck, C. W.; Ganske, J. A. “Detection of NOx in Automobile Exhaust: An Applied Experiment in
Atmospheric/Environmental Chemistry for the General Chemistry Laboratory,” Chem. Educator 2008, 13, 1–5.
Domínguez, A., Fernández, A.; González, N.; Iglesias, E.; Montenegro, L. “Determination of Critical Micelle Concentration of
Some Surfactants by Three Techniques,” J. Chem. Educ. 1997, 74, 1227–1231.
Gilbert, D. D. “Determining Optimum Spectral Bandwidth,” J. Chem. Educ. 1991, 68, A278–A281.
Han, J.; Story, T.; Han, G. “A Spectrophotometric Method for Quantitative Determination of Bromine Using Tris(2carboxyethyl)phophine,” J. Chem. Educ. 1999, 76, 976–977.
Higginbotham, C.; Pike, C. F.; Rice, J, K. “Spectroscopy in Sol-Gel Matricies,” J. Chem. Educ. 1998, 75, 461–464.
Hill, Z. D.; MacCarthy, P. “Novel Approach to Job’s Method,” J. Chem. Educ. 1986, 63, 162–167.
Ibañez, G. A.; Olivieri, A. C.; Escandar, G. M. “Determination of Equilibrium Constants of Metal Complexes from
Spectrophotometric Measurements,” J. Chem. Educ. 1999, 76, 1277–1281.
Long, J. R.; Drago, R. S. “The Rigorous Evaluation of Spectrophotometric Data to Obtain an Equilibrium Constant,” J. Chem.
Educ. 1982, 59, 1037–1039.
Lozano-Calero; D.; Martin-Palomeque, P. “Determination of Phosphorous in Cola Drinks,” J. Chem. Educ. 1996, 73, 1173–
1174.
Maloney, K. M.; Quiazon, E. M.; Indralingam, R. “Measurement of Iron in Egg Yolk: An Instrumental Analysis Measurement
Using Biochemical Principles,” J. Chem. Educ. 2008, 85, 399–400.
Mascotti, D. P.; Waner, M. J. “Complementary Spectroscopic Assays for Investigation Protein-Ligand Binding Activity: A
Project for the Advanced Chemistry Laboratory,” J. Chem. Educ. 2010, 87, 735–738.
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McDevitt, V. L.; Rodriquez, A.; Williams, K. R. “Analysis of Soft Drinks: UV Spectrophotometry, Liquid Chromatography, and
Capillary Electrophoresis,” J. Chem. Educ. 1998, 75, 625–629.
Mehra, M. C.; Rioux, J. “An Analytical Chemistry Experiment in Simultaneous Spectrophotometric Determination of Fe(III)
and Cu(II) with Hexacyanoruthenate(II) Reagent,” J. Chem. Educ. 1982, 59, 688–689.
Mitchell-Koch, J. T.; Reid, K. R.; Meyerhoff, M. E. “Salicylate Detection by Complexation with Iron(III) and Optical
Absorbance Spectroscopy,” J. Chem. Educ. 2008, 85, 1658–1659.
Msimanga, H. Z.; Wiese, J. “Determination of Acetaminophen in Analgesics by the Standard Addition Method: A Quantitative
Analytical Chemistry Laboratory,” Chem. Educator 2005, 10, 1–7.
Örstan, A.; Wojcik, J. F. “Spectroscopic Determination of Protein-Ligand Binding Constants,” J. Chem. Educ. 1987, 64, 814–
816.
Pandey, S.; Powell, J. R.; McHale, M. E. R.; Acree Jr., W. E. “Quantitative Determination of Cr(III) and Co(II) Using a
Spectroscopic H-Point Standard Addition,” J. Chem. Educ. 1997, 74, 848–850.
Parody-Morreale, A.; Cámara-Artigas, A.; Sánchez-Ruiz, J. M. “Spectrophotometric Determination of the Binding Constants of
Succinate and Chloride to Glutamic Oxalacetic Transaminase,” J. Chem. Educ. 1990, 67, 988–990.
Ravelo-Perez, L. M.; Hernández-Borges, J.; Rodríguez-Delgado, M. A.; Borges-Miquel, T. “Spectrophotometric Analysis of
Lycopene in Tomatoes and Watermelons: A Practical Class,” Chem. Educator 2008, 13, 1–3.
Russell, D. D.; Potts, J.; Russell, R. M.; Olson, C.; Schimpf, M. “Spectroscopic and Potentiometric Investigation of a Diprotic
Acid: An Experimental Approach to Understanding Alpha Functions,” Chem. Educator 1999, 4, 68–72.
Smith, E. T.; Matachek, J. R. “A Colorful Investigation of a Diprotic Acid: A General Chemistry Laboratory Exercise,” Chem.
Educator 2002, 7, 359–363
Tello-Solis, S. R. “Thermal Unfolding of Lysozyme Studied by UV Difference Spectroscopy,” Chem. Educator 2008, 13, 16–
18.
Tucker, S.; Robinson, R.; Keane, C.; Boff, M.; Zenko, M.; Batish, S.; Street, Jr., K. W. “Colorimetric Determination of pH,” J.
Chem. Educ. 1989, 66, 769–771.
Vitt, J. E. “Troubleshooting 101: An Instrumental Analysis Experiment,” J. Chem. Educ. 2008, 85, 1660–1662.
Williams, K. R.; Cole, S. R.; Boyette, S. E.; Schulman, S. G. “The Use of Dristan Nasal Spray as the Unknown for
Simultaneous Spectrophotometric Analysis of a Mixture,” J. Chem. Educ. 1990, 67, 535.
Walmsley, F. “Aggregation in Dyes: A Spectrophotometric Study,” J. Chem. Educ. 1992, 69, 583.
Wells, T. A. “Construction of a Simple Myoglobin-Based Optical Biosensor,” Chem. Educator 2007, 12, 1–3.
Yarnelle, M. K.; West, K. J. “Modification of an Ultraviolet Spectrophotometric Determination of the • Active Ingredients in
APC Tablets,” J. Chem. Educ. 1989, 66, 601–602.
IR Spectroscopy
Dragon, S.; Fitch, A. “Infrared Spectroscopy Determination of Lead Binding to Ethylenediaminetetraacetic Acid,” J. Chem.
Educ. 1998, 75, 1018–1021.
Frohlich, H. “Using Infrared Spectroscopy Measurements to Study Intermolecular Hydrogen Bonding,” J. Chem. Educ. 1993,
70, A3–A6.
Garizi, N.; Macias, A.; Furch, T.; Fan, R.; Wagenknecht, P.; Singmaster, K. A. “Cigarette Smoke Analysis Using an Inexpensive
Gas-Phase IR Cell,” J. Chem. Educ. 2001, 78, 1665–1666.
Indralingam, R.; Nepomuceno, A. I. “The Use of Disposable IR Cards for Quantitative Analysis Using an Internal Standard,” J.
Chem. Educ. 2001, 78, 958–960.
Mathias, L. J.; Hankins, M. G.; Bertolucci, C. M.; Grubb, T. L.; Muthiah, J. “Quantitative Analysis by FTIR: Thin Films of
Copolymers of Ethylene and Vinyl Acetate,” J. Chem. Educ. 1992, 69, A217–A219.
Schuttlefield, J. D.; Grassian, V. H. “ATR-FTIR Spectroscopy in the Undergraduate Chemistry Laboratory. Part I: Fundamentals
and Examples,” J. Chem. Educ. 2008, 85, 279–281.
Schuttlefield, J. D.; Larsen, S. C.; Grassian, V. H. “ATR-FTIR Spectroscopy in the Undergraduate Chemistry Laboratory. Part
II: A Physical Chemistry Laboratory Experiment on Surface Adsorption,” J. Chem. Educ. 2008, 85, 282–284.
Seasholtz, M. B.; Pence, L. E.; Moe Jr., O. A. “Determination of Carbon Monoxide in Automobile Exhaust by FTIR
Spectroscopy,” J. Chem. Educ. 1988, 65, 820–823.
Atomic Absorption and Atomic Emission Spectroscopy
Amarasiriwardena, D. “Teaching analytical atomic spectroscopy advances in an environmental chemistry class using a projectbased laboratory approach: investigation of lead and arsenic distributions in a lead arsenate contaminated apple orchard,” Anal.
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Bioanal. Chem. 2007, 388, 307–314.
Buffen, B. P. “Removal of Heavy Metals from Water: An Environmentally Significant Atomic Absorption Spectrometry
Experiment,” J. Chem. Educ. 1999, 76, 1678–1679.
Dockery, C. R.; Blew, M. J.; Goode, S. R. “Visualizing the Solute Vaporization Interference in Flame Atomic Absorption
Spectroscopy,” J. Chem. Educ. 2008, 85, 854–858.
Donas, M. K.; Whissel, G.; Dumas, A.; Golden, K. “Analyzing Lead Content in Ancient Bronze Coins by Flame Atomic
Absorption Spectroscopy,” J. Chem. Educ. 2009, 86, 343–346.
Gilles de Pelichy, L. D.; Adams, C.; Smith, E. T. “Analysis of the Essential Nutrient Strontium in Marine Aquariums by Atomic
Absorption Spectroscopy,” J. Chem. Educ. 1997, 74, 1192–1194.
Hoskins, L. C.; Reichardt, P. B.; Stolzberg, R. J. “Determination of the Extraction Constant for Zinc Pyrrolidinecarbodithioate,”
J. Chem. Educ. 1981, 58, 580–581.
Kooser, A. S.; Jenkins, J. L.; Welch, L. E. “Inductively Coupled Plasma-Atomic Emission Spectroscopy: Two Laboratory
Activities for the Undergraduate Instrumental Analysis Course,” J. Chem. Educ. 2003, 80, 86–88.
Kostecka, K. S. “Atomic Absorption Spectroscopy of Calcium in Foodstuffs in Non-Science-Major Courses,” J. Chem. Educ.
2000, 77, 1321–1323.
Lehman, T. A.; Everett, W. W. “Solubility of Lead Sulfate in Water and in Sodium Sulfate Solutions,” J. Chem. Educ. 1982, 59,
797.
Markow, P. G. “Determining the Lead Content of Paint Chips,” J. Chem. Educ. 1996, 73, 178–179.
Masina, M. R.; Nkosi, P. A.; Rasmussen, P. W.; Shelembe, J. S.; Tyobeka, T. E. “Determination of Metal Ions in Pineapple Juice
and Effluent of a Fruit Canning Industry,” J. Chem. Educ. 1989, 66, 342–343.
Quigley, M. N. “Determination of Calcium in Analgesic Tablets using Atomic Absorption Spectrophotometry,” J. Chem. Educ.
1994, 71, 800.
Quigley, M. N.; Vernon, F. “Determination of Trace Metal Ion Concentrations in Seawater,” J. Chem. Educ. 1996, 73, 671–675.
Quigley, M. N.; Vernon, F. “A Matrix Modification Experiment for Use in Electrothermal Atomic Absorption
Spectrophotometry,” J. Chem. Educ. 1996, 73, 980–981.
Rheingold, A. L.; Hues, S.; Cohen, M. N. “Strontium and Zinc Content in Bones as an Indication of Diet,” J. Chem. Educ.
1983, 60, 233–234.
Rocha, F. R. P.; Nóbrega, J. A. “Effects of Solution Physical Properties on Copper and Chromium Signals in Flame Atomic
Absorption Spectrometry,” J. Chem. Educ. 1996, 73, 982–984.
Fluorescence and Phosphorescence Spectroscopy
Buccigross, J. M.; Bedell, C. M.; Suding-Moster, H. L. “Fluorescent Measurement of TNS Binding to Calmodulin,” J. Chem.
Educ. 1996, 73, 275–278.
Henderleiter, J. A.; Hyslopo, R. M. “The Analysis of Riboflavin in Urine by Fluorescence,” J. Chem. Educ. 1996, 73, 563–564.
Lagoria, M. G.; Román, E. S. “How Does Light Scattering Affect Luminescence? Fluorescence Spectra and Quantum Yields in
the Solid Form,” J. Chem. Educ. 2002, 79, 1362–1367.
Richardson, D. P.; Chang, R. “Lecture Demonstrations of Fluorescence and Phosphorescence,” Chem. Educator 2007, 12, 272–
274.
Seixas de Melo, J. S.; Cabral, C.; Burrows, H. D. “Photochemistry and Photophysics in the Laboratory. Showing the Role of
Radiationless and Radiative Decay of Excited States,” Chem. Educator 2007, 12, 1–6.
Sheffield, M. C.; Nahir, T. M. “Analysis of Selenium in Brazil Nuts by Microwave Digestion and Fluorescence Detection,” J.
Chem. Educ. 2002, 79, 1345–1347.
Signal Averaging
Blitz, J. P.; Klarup, D. G. “Signal-to-Noise Ratio, Signal Processing, and Spectral Information in the Instrumental Analysis
Laboratory,” J. Chem. Educ. 2002, 79, 1358–1360.
Stolzberg, R. J. “Introduction to Signals and Noise in an Instrumental Method Course,” J. Chem. Educ. 1983, 60, 171–172.
Tardy, D. C. “Signal Averaging. A Signal-to-Noise Enhancement Experiment for the Advanced Chemistry Laboratory,” J.
Chem. Educ. 1986, 63, 648–650.
The following sources provide additional information on spectroscopy in the following areas: general spectroscopy, Beer’s law,
instrumentation, Fourier transforms, , IR spectroscopy, atomic absorption and emission, luminescence, and applications.
General Spectroscopy
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Ball, D. W. “Units! Units! Units!” Spectroscopy 1995, 10(8), 44–47.
A History of Analytical Chemistry, Laitinen, H. A.; Ewing, G. W, Eds. The Division of Analytical Chemistry of the American
Chemical Society: Washington, D. C., 1977, p103–243.
Ingle, J. D.; Crouch, S. R. Spectrochemical Analysis, Prentice Hall, Englewood Cliffs, N. J.; 1988.
Macomber, R. S. “A Unifying Approach to Absorption Spectroscopy at the Undergraduate Level,” J. Chem. Educ. 1997, 74,
65–67.
Orchin, M.; Jaffe, H. H. Symmetry, Orbitals and Spectra, Wiley-Interscience: New York, 1971.
Thomas, N. C. “The Early History of Spectroscopy,” J. Chem. Educ. 1991, 68, 631–633.
Beer’s Law
Lykos, P. “The Beer-Lambert Law Revisited: A Development without Calculus,” J. Chem. Educ. 1992, 69, 730–732.
Ricci, R. W.; Ditzler, M. A.; Nestor, L. P. “Discovering the Beer-Lambert Law,” J. Chem. Educ. 1994, 71, 983–985.
Instrumentation
Altermose, I. R. “Evolution of Instrumentation for UV-Visible Spectrophotometry: Part I,” J. Chem. Educ. 1986, 63, A216–
A223.
Altermose, I. R. “Evolution of Instrumentation for UV-Visible Spectrophotometry: Part II,” J. Chem. Educ. 1986, 63, A262–
A266.
Grossman, W. E. L. “The Optical Characteristics and Production of Diffraction Gratings,” J. Chem. Educ. 1993, 70, 741–748.
Jones, D. G. “Photodiode Array Detectors in UV-Vis Spectroscopy: Part I,” Anal. Chem. 1985, 57, 1057A–1073A.
Jones, D. G. “Photodiode Array Detectors in UV-Vis Spectroscopy: Part II,” Anal. Chem. 1985, 11, 1207A–1214A.
Palmer, C. “Diffraction Gratings,” Spectroscopy, 1995, 10(2), 14–15.
Fourier Transforms
Bracewell, R. N. “The Fourier Transform,” Sci. American 1989, 260(6), 85–95.
Glasser, L. “Fourier Transforms for Chemists: Part I. Introduction to the Fourier Transform,” J. Chem. Educ. 1987, 64, A228–
A233.
Glasser, L. “Fourier Transforms for Chemists: Part II. Fourier Transforms in Chemistry and Spectroscopy,” J. Chem. Educ.
1987, 64, A260–A266.
Glasser, L. “Fourier Transforms for Chemists: Part III. Fourier Transforms in Data Treatment,” J. Chem. Educ. 1987, 64, A306–
A313.
Graff, D. K. “Fourier and Hadamard: Transforms in Spectroscopy,” J. Chem. Educ. 1995, 72, 304–309.
Griffiths, P. R. Chemical Fourier Transform Spectroscopy, Wiley-Interscience: New York, 1975.
Transform Techniques in Chemistry, Griffiths, P. R. Ed., Plenum Press: New York, 1978.
Perkins, W. E. “Fourier Transform Infrared Spectroscopy: Part I. Instrumentation,” J. Chem. Educ. 1986, 63, A5–A10.
Perkins, W. E. “Fourier Transform Infrared Spectroscopy: Part II. Advantages of FT-IR,” J. Chem. Educ. 1987, 64, A269–
A271.
Perkins, W. E. “Fourier Transform Infrared Spectroscopy: Part III. Applications,” J. Chem. Educ. 1987, 64, A296–A305.
Strong III, F. C. “How the Fourier Transform Infrared Spectrophotometer Works,” J. Chem. Educ. 1979, 56, 681–684.
IR Spectroscopy
Optical Spectroscopy: Sampling Techniques Manual, Harrick Scientific Corporation: Ossining, N. Y., 1987.
Leyden, D. E.; Shreedhara Murthy, R. S. “Surface-Selective Sampling Techniques in Fourier Transform Infrared Spectroscopy,”
Spectroscopy 1987, 2(2), 28–36.
Porro, T. J.; Pattacini, S. C. “Sample Handling for Mid-Infrared Spectroscopy, Part I: Solid and Liquid Sampling,” Spectroscopy
1993, 8(7), 40–47.
Porro, T. J.; Pattacini, S. C. “Sample Handling for Mid-Infrared Spectroscopy, Part II: Specialized Techniques,” Spectroscopy
1993, 8(8), 39–44.
Atomic Absorption and Emission
Blades, M. W.; Weir, D. G. “Fundamental Studies of the Inductively Coupled Plasma,” Spectroscopy 1994, 9, 14–21.
Greenfield, S. “Invention of the Annular Inductively Coupled Plasma as a Spectroscopic Source,” J. Chem. Educ. 2000, 77,
584–591.
Hieftje, G. M. “Atomic Absorption Spectrometry - Has it Gone or Where is it Going?” J. Anal. At. Spectrom. 1989, 4, 117–122.
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Jarrell, R. F. “A Brief History of Atomic Emission Spectrochemical Analysis, 1666-1950,” J. Chem. Educ. 2000, 77, 573–576
Koirtyohann, S. R. “A History of Atomic Absorption Spectrometry From an Academic Perspective,” Anal. Chem. 1991, 63,
1024A–1031A.
L’Vov, B. V. “Graphite Furnace Atomic Absorption Spectrometry,” Anal. Chem. 1991, 63, 924A–931A.
Slavin, W. “A Comparison of Atomic Spectroscopic Analytical Techniques,” Spectroscopy, 1991, 6, 16–21.
Van Loon, J. C. Analytical Atomic Absorption Spectroscopy, Academic Press: New York, 1980.
Walsh, A. “The Development of Atomic Absorption Methods of Elemental Analysis 1952-1962,” Anal. Chem. 1991, 63, 933A–
941A.
Welz, B. Atomic Absorption Spectroscopy, VCH: Deerfield Beach, FL, 1985.
Luminescence Spectroscopy
Guilbault, G. G. Practical Fluorescence, Decker: New York, 1990.
Schenk, G. “Historical Overview of Fluorescence Analysis to 1980,” Spectroscopy 1997, 12, 47–56.
Vo-Dinh, T. Room-Temperature Phosphorimetry for Chemical Analysis, Wiley-Interscience: New York, 1984.
Winefordner, J. D.; Schulman, S. G.; O’Haver, T. C. Luminescence Spectroscopy in Analytical Chemistry, Wiley-Interscience:
New York, 1969.
Applications
Trace Analysis and Spectroscopic Methods for Molecules, Christian, G. D.; Callis, J. B. Eds., Wiley-Interscience: New York,
1986.
Vandecasteele, C.; Block, C. B. Modern Methods for Trace Element Determination, Wiley: Chichester, England, 1994.
Skoog, D. A.; Holler, F. J.; Nieman, T. A. Principles of Instrumental Analysis, Saunders: Philadelphia, 1998.
Van Loon, J. C. Selected Methods of Trace Metal Analysis: Biological and Environmental Samples, Wiley-Interscience: New
York, 1985.
Gathered here are resources and experiments for analyzing multicomponent samples using mathematical techniques not covered in
this textbook.
Aberasturi, F.; Jimenez, A. I.; Jimenez, F.; Arias, J. J. “UV-Visible First-Derivative Spectrophotometry Applied to an Analysis
of a Vitamin Mixture,” J. Chem. Educ. 2001, 78, 793–795.
Afkhami, A.; Abbasi-Tarighat, M.; Bahram, M.; Abdollahi, H. “A new strategy for solving matrix effect in multivariate
calibration standard addition data using combination of H-point curve isolation and H-point standard addition methods,” Anal.
Chim. Acta 2008, 613, 144–151.
Brown, C. W.; Obremski, R. J. “Multicomponent Quantitative Analysis,” Appl. Spectrosc. Rev. 1984, 20, 373–418.
Charles, M. J.; Martin, N. W.; Msimanga, H. Z. “Simultaneous Determination of Aspirin, Salicylamide, and Caffeine in Pain
Relievers by Target Factor Analysis,” J. Chem. Educ. 1997, 74, 1114–1117.
Dado, G.; Rosenthal, J. “Simultaneous Determination of Cobalt, Copper, and Nickel by Multivariate Linear Regression,” J.
Chem. Educ. 1990, 67, 797–800.
DiTusa, M. R.; Schilt, A. A. “Selection of Wavelengths for Optimum Precision in Simultaneous Spectrophotometric
Determinations,” J. Chem. Educ. 1985, 62, 541–542.
Gómez, D. G.; de la Peña, A. M.; Mansilla, A. E.; Olivieri, A. C. “Spectrophotometric Analysis of Mixtures by Classical LeastSquares Calibration: An Advanced Experiment Introducing MATLAB,” Chem. Educator 2003, 8, 187–191.
Harvey, D. T.; Bowman, A. “Factor Analysis of Multicomponent Samples,” J. Chem. Educ. 1990, 67, 470–472.
Lucio-Gutierrez, J. R.; Salazar-Cavazos, M. L.; de Torres, N. W. “Chemometrics in the Teaching Lab. Quantification of a
Ternary Mixture of Common Pharmaceuticals by First- and Second-Derivative IR Spectroscopy,” Chem. Educator 2004, 9,
234–238.
Padney, S.; McHale, M. E. R.; Coym, K. S.; Acree Jr., W. E. “Bilinear Regression Analysis as a Means to Reduce Matrix
Effects in Simultaneous Spectrophotometric Determination of Cr(III) and Co(II),” J. Chem. Educ. 1998, 75, 878–880.
Raymond, M.; Jochum, C.; Kowalski, B. R. “Optimal Multicomponent Analysis Using the Generalized Standard Addition
Method,” J. Chem. Educ. 1983, 60, 1072–1073.
Ribone, M. E.; Pagani, A. P.; Olivieri, A. C.; Goicoechea, H. C. “Determination of the Active Principle in a Spectrophotometry
and Principal Component Regression Analysis,” J. Chem. Educ. 2000, 77, 1330–1333.
Rojas, F. S.; Ojeda, C. B. “Recent developments in derivative ultraviolet/visible absorption spectrophotometry: 2004-2008,”
Anal. Chim. Acta 2009, 635, 22–44.
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Chapter 11
The following set of experiments introduce students to the applications of electrochemistry. Experiments are grouped into four
categories: general electrochemistry, preparation of electrodes, potentiometry, coulometry, and voltammetry and amperometry.
General Electrochemistry
Mills, K. V.; Herrick, R. S.; Guilmette, L. W.; Nestor, L. P.; Shafer, H.; Ditzler, M. A. “Introducing Undergraduate Students to
Electrochemistry: A Two-Week Discovery Chemistry Experiment,” J. Chem. Educ. 2008, 85, 1116–119.
Preparation of Electrodes
Christopoulos, T. K.; Diamandis, E. P. “Use of a Sintered Glass Crucible for Easy Construction of Liquid-Membrane IonSelective Electrodes,” J. Chem. Educ. 1988, 65, 648.
Fricke, G. H.; Kuntz, M. J. “Inexpensive Solid-State Ion-Selective Electrodes for Student Use,” J. Chem. Educ. 1977, 54, 517–
520.
Inamdar, S. N.; Bhat, M. A.; Haram, S. K. “Construction of Ag/AgCl Reference Electrode form Used Felt-Tipped Pen Barrel
for Undergraduate Laboratory,” J. Chem. Educ. 2009, 86, 355–356.
Lloyd, B. W.; O’Brien, F. L.; Wilson, W. D. “Student Preparation and Analysis of Chloride and Calcium Ion Selective
Electrodes,” J. Chem. Educ. 1976, 53, 328–330.
Mifflin, T. E.; Andriano, K. M.; Robbins, W. B. “Determination of Penicillin Using an Immobilized Enzyme Electrode,” J.
Chem. Educ. 1984, 61, 638–639.
Palanivel, A.; Riyazuddin, P. “Fabrication of an Inexpensive Ion-Selective Electrode,” J. Chem. Educ. 1984, 61, 290.
Ramaley, L; Wedge, P. J.; Crain, S. M. “Inexpensive Instrumental Analysis: Part 1. Ion-Selective Electrodes,” J. Chem. Educ.
1994, 71, 164–167.
Selig, W. S. “Potentiometric Titrations Using Pencil and Graphite Sensors,” J. Chem. Educ. 1984, 61, 80–81.
Potentiometry
Chan, W. H; Wong, M. S.; Yip, C. W. “Ion-Selective Electrode in Organic Analysis: A Salicylate Electrode,” J. Chem. Educ.
1986, 63, 915–916.
Harris, T. M. “Potentiometric Measurement in a Freshwater Aquarium,” J. Chem. Educ. 1993, 70, 340–341.
Kauffman, C. A.; Muza, A. L.; Porambo, M. W.; Marsh, A. L. “Use of a Commercial Silver-Silver Chloride Electrode for the
Measurement of Cell Potentials to Determine Mean Ionic Activity Coefficients,” Chem. Educator 2010, 15, 178–180.
Martínez-Fàbregas, E.; Alegret, S. “A Practical Approach to Chemical Sensors through Potentiometric Transducers:
Determination of Urea in Serum by Means of a Biosensor,” J. Chem. Educ. 1994, 71, A67–A70.
Moresco, H.; Sansón, P.; Seoane, G. “Simple Potentiometric Determination of Reducing Sugars,” J. Chem. Educ. 2008, 85,
1091–1093.
Radic, N.; Komijenovic, J. “Potentiometric Determination of an Overall Formation Constant Using an Ion-Selective Membrane
Electrode,” J. Chem. Educ. 1993, 70, 509–511.
Riyazuddin, P.; Devika, D. “Potentiometric Acid–Base Titrations with Activated Graphite Electrodes,” J. Chem. Educ. 1997,
74, 1198–1199.
Coulometry
Bertotti, M.; Vaz, J. M.; Telles, R. “Ascorbic Acid Determination in Natural Orange Juice,” J. Chem. Educ. 1995, 72, 445–447.
Kalbus, G. E.; Lieu, V. T. “Dietary Fat and Health: An Experiment on the Determination of Iodine Number of Fats and Oils by
Coulometric Titration,” J. Chem. Educ. 1991, 68, 64–65.
Lötz, A. “A Variety of Electrochemical Methods in a Coulometric Titration Experiment,” J. Chem. Educ. 1998, 75, 775–777.
Swim, J.; Earps, E.; Reed, L. M.; Paul, D. “Constant-Current Coulometric Titration of Hydrochloric Acid,” J. Chem. Educ.
1996, 73, 679–683.
Voltammetry and Amperometry
Blanco-López, M. C.; Lobo-Castañón, M. J.; Miranda-Ordieres, A. J. “Homemade Bienzymatic-Amperometric Biosensor for
Beverages Analysis,” J. Chem. Educ. 2007, 84, 677–680.
García-Armada, P.; Losada, J.; de Vicente-Pérez, S. “Cation Analysis Scheme by Differential Pulse Polarography,” J. Chem.
Educ. 1996, 73, 544–547.
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Herrera-Melián, J. A.; Doña-Rodríguez, J. M.; Hernández-Brito, J.; Pérez-Peña, J. “Voltammetric Determination of Ni and Co
in Water Samples,” J. Chem. Educ. 1997, 74, 1444–1445.
King, D.; Friend, J.; Kariuki, J. “Measuring Vitamin C Content of Commercial Orange Juice Using a Pencil Lead Electrode,” J.
Chem. Educ. 2010, 87, 507–509.
Marin, D.; Mendicuti, F. “Polarographic Determination of Composition and Thermodynamic Stability Constant of a Complex
Metal Ion,” J. Chem. Educ. 1988, 65, 916–918.
Sadik, O. A.; Brenda, S.; Joasil, P.; Lord, J. “Electropolymerized Conducting Polymers as Glucose Sensors,” J. Chem. Educ.
1999, 76, 967–970.
Sittampalam, G.; Wilson, G. S. “Amperometric Determination of Glucose at Parts Per Million Levels with Immobilized
Glucose Oxidase,” J. Chem. Educ. 1982, 59, 70–73.
Town, J. L.; MacLaren, F.; Dewald, H. D. “Rotating Disk Voltammetry Experiment,” J. Chem. Educ. 1991, 68, 352–354.
Wang, J. “Sensitive Electroanalysis Using Solid Electrodes,” J. Chem. Educ. 1982, 59, 691–692.
Wang, J. “Anodic Stripping Voltammetry,” J. Chem. Educ. 1983, 60, 1074–1075.
Wang, J.; Maccà, C. “Use of Blood-Glucose Test Strips for Introducing Enzyme Electrodes and Modern Biosensors,” J. Chem.
Educ. 1996, 73, 797–800.
Wang, Q.; Geiger, A.; Frias, R; Golden, T. D. “An Introduction to Electrochemistry for Undergraduates: Detection of Vitamin C
(Ascorbic Acid) by Inexpensive Electrode Sensors,” Chem. Educator 2000, 5, 58–60.
The following general references providing a broad introduction to electrochemistry.
Adams, R. N. Electrochemistry at Solid Surfaces, Marcel Dekker: New York, 1969.
Bard, A. J.; Faulkner, L. R. Electrochemical Methods, Wiley: New York, 1980.
Faulkner, L. R. “Electrochemical Characterization of Chemical Systems” in Kuwana, T. E., ed. Physical Methods in Modern
Chemical Analysis, Vol. 3, Academic Press: New York, 1983, pp. 137–248.
Kissinger, P. T.; Heineman, W. R. Laboratory Techniques in Electroanalytical Chemistry, Marcel Dekker: New York, 1984.
Lingane, J. J. Electroanalytical Chemistry, 2nd Ed., Interscience: New York, 1958.
Sawyer, D. T.; Roberts, J. L., Jr. Experimental Electrochemistry for Chemists, Wiley-Interscience: New York, 1974.
Vassos, B. H.; Ewing, G. W. Electroanalytical Chemistry, Wiley-Interscience: New York, 1983.
These short articles provide a good introduction to important principles of electrochemistry.
Faulkner, L. R. “Understanding Electrochemistry: Some Distinctive Concepts,” J. Chem. Educ. 1983, 60, 262–264.
Huddle, P. A.; White, M. D.; Rogers, F. “Using a Teaching Model to Correct Known Misconceptions in Electrochemistry,” J.
Chem. Educ. 2000, 77, 104–110.
Maloy, J. T. “Factors Affecting the Shape of Current-Potential Curves,” J. Chem. Educ. 1983, 60, 285–289.
Thompson, R. Q.; Craig, N. C. “Unified Electroanalytical Chemistry: Application of the Concept of Equilibrium,” J. Chem.
Educ. 2001, 78, 928–934.
Zoski, C. G. “Charging Current Discrimination in Analytical Voltammetry,” J. Chem. Educ. 1986, 63, 910–914.
Additional information on potentiometry and ion-selective electrodes can be found in the following sources.
Bakker, E.; Diamond, D.; Lewenstam, A.; Pretsch, E. “Ions Sensors: Current Limits and New Trends,” Anal. Chim. Acta 1999,
393, 11–18.
Bates, R. G. Determination of pH: Theory and Practice, 2nd ed., Wiley: New York, 1973.
Buck, R. P. “Potentiometry: pH Measurements and Ion Selective Electrodes” in Weissberger, A., ed. Physical Methods of
Organic Chemistry, Vol. 1, Part IIA, Wiley: New York, 1971, pp. 61–162.
Cammann, K. Working With Ion-Selective Electrodes, Springer-Verlag: Berlin, 1977.
Evans, A. Potentiometry and Ion-Selective Electrodes, Wiley: New York, 1987.
Frant, M. S. “Where Did Ion Selective Electrodes Come From?” J. Chem. Educ. 1997, 74, 159–166.
Light, T. S. “Industrial Use and Application of Ion-Selective Electrodes,” J. Chem. Educ. 1997, 74, 171–177.
Rechnitz, G. A. “Ion and Bio-Selective Membrane Electrodes,” J. Chem. Educ. 1983, 60, 282–284.
Ruzicka, J. “The Seventies—Golden Age for Ion-Selective Electrodes,” J. Chem. Educ. 1997, 74, 167–170.
Young, C. C. “Evolution of Blood Chemistry Analyzers Based on Ion Selective Electrodes,” J. Chem. Educ. 1997, 74, 177–182.
The following sources provide additional information on electrochemical biosensors.
Alvarez-Icasa, M.; Bilitewski, U. “Mass Production of Biosensors,” Anal. Chem. 1993, 65, 525A–533A.
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Meyerhoff, M. E.; Fu, B.; Bakker, E. Yun, J-H; Yang, V. C. “Polyion-Sensititve Membrane Electrodes for Biomedical
Analysis,” Anal. Chem. 1996, 68, 168A–175A.
Nicolini, C.; Adami, M; Antolini, F.; Beltram, F.; Sartore, M.; Vakula, S. “Biosensors: A Step to Bioelectronics,” Phys. World,
May 1992, 30–34.
Rogers, K. R.; Williams. L. R. “Biosensors for Environmental Monitoring: A Regulatory Perspective,” Trends Anal. Chem.
1995, 14, 289–294.
Schultz, J. S. “Biosensors,” Sci. Am. August 1991, 64–69.
Thompson, M.; Krull, U. “Biosensors and the Transduction of Molecular Recognition,” Anal. Chem. 1991, 63, 393A–405A.
Vadgama, P. “Designing Biosensors,” Chem. Brit. 1992, 28, 249–252.
A good source covering the clinical application of electrochemistry is listed below.
Wang, J. Electroanalytical Techniques in Clinical Chemistry and Laboratory Medicine, VCH: New York, 1998.
Coulometry is covered in the following texts.
Rechnitz, G. A. Controlled-Potential Analysis, Macmillan: New York, 1963.
Milner, G. W. C.; Philips, G. Coulometry in Analytical Chemistry, Pergamon: New York, 1967.
For a description of electrogravimetry, see the following resource.
Tanaka, N. “Electrodeposition”, in Kolthoff, I. M.; Elving, P. J., eds. Treatise on Analytical Chemistry, Part I: Theory and
Practice, Vol. 4, Interscience: New York, 1963.
The following sources provide additional information on polarography and pulse polarography.
Flato, J. B. “The Renaissance in Polarographic and Voltammetric Analysis,” Anal. Chem. 1972, 44(11), 75A–87A.
Kolthoff, I. M.; Lingane, J. J. Polarography, Interscience: New York, 1952.
Osteryoung, J. “Pulse Voltammetry,” J. Chem. Educ. 1983, 60, 296–298.
Additional Information on stripping voltammetry is available in the following text.
Wang, J. Stripping Analysis, VCH Publishers: Deerfield Beach, FL, 1985.
The following papers discuss the numerical simulation of voltammetry.
Bozzini, B. “A Simple Numerical Procedure for the Simulation of “Lifelike” Linear-Sweep Voltammograms,” J. Chem. Educ.
2000, 77, 100–103.
Howard, E.; Cassidy, J. “Analysis with Microelectrodes Using Microsoft Excel Solver,” J. Chem. Educ. 2000, 77, 409–411.
Gathered together here are many useful resources for cyclic voltammetry, including experiments.
Carriedo, G. A. “The Use of Cyclic Voltammetry in the Study of the Chemistry of Metal–Carbonyls,” J. Chem. Educ. 1988, 65,
1020–1022.
García-Jareño, J. J.; Benito, D.; Navarro-Laboulais, J.; Vicente, F. “Electrochemical Behavior of Electrodeposited Prussian Blue
Films on ITO Electrodes,” J. Chem. Educ. 1998, 75, 881–884.
Gilles de Pelichy, L. D.; Smith, E. T. “A Study of the Oxidation Pathway of Adrenaline by Cyclic Voltammetry,” Chem.
Educator 1997, 2(2), 1–13.
Gomez, M. E.; Kaifer, A. E. “Voltammetric Behavior of a Ferrocene Derivative,” J. Chem. Educ. 1992, 69, 502–505.
Heffner, J. E.; Raber, J. C.; Moe, O. A.; Wigal, C. T. “Using Cyclic Voltammetry and Molecular Modeling to Determine
Substituent Effects in the One-Electron Reduction of Benzoquinones,” J. Chem. Educ. 1998, 75, 365–367.
Heinze, J. “Cyclic Voltammetry—Electrochemical Spectroscopy,” Angew. Chem, Int. Ed. Eng. 1984, 23, 831–918.
Holder, G. N.; Farrar, D. G.; McClure, L. L. “Voltammetric Reductions of Ring-Substituted Acetophenones. 1. Determination of
an Electron-Transfer Mechanism Using Cyclic Voltammetry and Computer Modeling: The Formation and Fate of a Radical
Anion,” Chem. Educator 2001, 6, 343–349.
Ibanez, J. G.; Gonzalez, I.; Cardenas, M. A. “The Effect of Complex Formation Upon the Redox Potentials of Metal Ions:
Cyclic Voltammetry Experiments,” J. Chem. Educ. 1988, 65, 173–175.
Ito, T.; Perara, D. M. N. T.; Nagasaka, S. “Gold Electrodes Modified with Self-Assembled Monolayers for Measuring LAscobric acid,” J. Chem. Educ. 2008, 85, 1112–1115.
Kissinger, P. T.; Heineman, W. R. “Cyclic Voltammetry,” J. Chem. Educ. 1983, 60, 702–706.
Mabbott, G. A. “An Introduction to Cyclic Voltammetry,” J. Chem. Educ. 1983, 60, 697–702.
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Petrovic, S. “Cyclic Voltammetry of Hexachloroiridate (IV): An Alternative to the Electrochemical Study of the Ferricyanide
Ion,” Chem. Educator 2000, 5, 231–235.
Toma, H. E.; Araki, K.; Dovidauskas, S. “A Cyclic Voltammetry Experiment Illustrating Redox Potentials, Equilibrium
Constants and Substitution Reaction in Coordination Chemistry,” J. Chem. Educ. 2000, 77, 1351–1353.
Walczak, M. W.; Dryer, D. A.; Jacobson, D. D,; Foss, M. G.; Flynn, N. T. “pH-Dependent Redox Couple: Illustrating the Nernst
Equation Using Cyclic Voltammetry,” J. Chem. Educ. 1997, 74, 1195–1197.
Chapter 12
The following set of experiments introduce students to the applications of chromatography and electrophoresis. Experiments are
grouped into five categories: gas chromatography, high-performance liquid chromatography, ion-exchange chromatography, sizeexclusion chromatography, and electrophoresis.
Gas Chromatography
Bishop, R. D., Jr. “Using GC–MS to Determine Relative Reactivity Ratios,” J. Chem. Educ. 1995, 72, 743–745.
Elderd, D. M.; Kildahl, N. K.; Berka, L. H. “Experiments for Modern Introductory Chemistry: Identification of Arson
Accelerants by Gas Chromatography,” J. Chem. Educ. 1996, 73, 675–677.
Fleurat-Lessard, P.; Pointet, K.; Renou-Gonnord, M.-F. “Quantitative Determination of PAHs in Diesel Engine Exhausts by
GC–MS,” J. Chem. Educ. 1999, 76, 962–965.
Galipo, R. C.; Canhoto, A. J.; Walla, M. D.; Morgan, S. L. “Analysis of Volatile Fragrance and Flavor Compounds by
Headspace Solid Phase Microextraction and GC–MS,” J. Chem. Educ. 1999, 76, 245–248.
Graham, R. C.; Robertson, J. K. “Analysis of Trihalomethanes in Soft Drinks,” J. Chem. Educ. 1988, 65, 735–737.
Heinzen, H.; Moyan, P.; Grompone, A. “Gas Chromatographic Determination of Fatty Acid Compositions,” J. Chem. Educ.
1985, 62, 449–450.
Kegley, S. E.; Hansen, K. J.; Cunningham, K. L. “Determination of Polychlorinated Biphenyls (PCBs) in River and Bay
Sediments,” J. Chem. Educ. 1996, 73, 558–562.
Kostecka, K. S.; Rabah, A.; Palmer, C. F., Jr. “GC/MS Analysis of the Aromatic Composition of Gasoline,” J. Chem. Educ.
1995, 72, 853–854.
Quach, D. T.; Ciszkowski, N. A.; Finlayson-Pitts, B. J. “A New GC-MS Experiment for the Undergraduate Instrumental
Analysis Laboratory in Environmental Chemistry: Methyl-t-butyl Ether and Benzene in Gasoline,” J. Chem. Educ. 1998, 75,
1595–1598.
Ramachandran, B. R.; Allen, J. M.; Halpern, A. M. “Air–Water Partitioning of Environmentally Important Organic
Compounds,” J. Chem. Educ. 1996, 73, 1058–1061.
Rice, G. W. “Determination of Impurities in Whiskey Using Internal Standard Techniques,” J. Chem. Educ. 1987, 64, 1055–
1056.
Rubinson, J. F.; Neyer-Hilvert, J. “Integration of GC-MS Instrumentation into the Undergraduate Laboratory: Separation and
Identification of Fatty Acids in Commercial Fats and Oils,” J. Chem. Educ. 1997, 74, 1106–1108.
Rudzinski, W. E.; Beu, S. “Gas Chromatographic Determination of Environmentally Significant Pesticides,” J. Chem. Educ.
1982, 59, 614–615.
Sobel, R. M.; Ballantine, D. S.; Ryzhov, V. “Quantitation of Phenol Levels in Oil of Wintergreen Using Gas Chromatography–
Mass Spectrometry with Selected Ion Monitoring,” J. Chem. Educ. 2005, 82, 601–603.
Welch, W. C.; Greco, T. G. “An Experiment in Manual Multiple Headspace Extraction for Gas Chromatography,” J. Chem.
Educ. 1993, 70, 333–335.
Williams, K. R.; Pierce, R. E. “The Analysis of Orange Oil and the Aqueous Solubility of d-Limone,” J. Chem. Educ. 1998, 75,
223–226.
Wong, J. W.; Ngim, K. K.; Shibamoto, T.; Mabury, S. A.; Eiserich, J. P.; Yeo, H. C. H. “Determination of Formaldehyde in
Cigarette Smoke,” J. Chem. Educ. 1997, 74, 1100–1103.
Yang, M. J.; Orton, M. L., Pawliszyn, J. “Quantitative Determination of Caffeine in Beverages Using a Combined SPMEGC/MS Method,” J. Chem. Educ. 1997, 74, 1130–1132.
High-Performance Liquid Chromatography
Batchelor, J. D.; Jones, B. T. “Determination of the Scoville Heat Value for Hot Sauces and Chilies: An HPLC Experiment,” J.
Chem. Educ. 2000, 77, 266–267.
Beckers, J. L. “The Determination of Caffeine in Coffee: Sense or Nonsense?” J. Chem. Educ. 2004, 81, 90–93.
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Betts, T. A. “Pungency Quantitation of Hot Pepper Sauces Using HPLC,” J. Chem. Educ. 1999, 76, 240–244.
Bidlingmeyer, B. A.; Schmitz, S. “The Analysis of Artificial Sweeteners and Additives in Beverages by HPLC,” J. Chem. Educ.
1991, 68, A195–A200.
Bohman, O.; Engdahl, K.-A.; Johnsson, H. “High Performance Liquid Chromatography of Vitamin A: A Quantitative
Determination,” J. Chem. Educ. 1982, 59, 251–252.
Brenneman, C. A.; Ebeler, S. E. “Chromatographic Separations Using Solid-Phase Extraction Cartridges: Separation of Wine
Phenolics,” J. Chem. Educ. 1999, 76, 1710–1711.
Cantwell, F. F.; Brown, D. W. “Liquid Chromatographic Determination of Nitroanilines,” J. Chem. Educ. 1981, 58, 820–823.
DiNunzio, J. E. “Determination of Caffeine in Beverages by High Performance Liquid Chromatography,” J. Chem. Educ. 1985,
62, 446–447.
Ferguson, G. K. “Quantitative HPLC Analysis of an Analgesic/Caffeine Formulation: Determination of Caffeine,” J. Chem.
Educ. 1998, 75, 467–469.
Ferguson, G. K. “Quantitative HPLC Analysis of a Psychotherapeutic Medication: Simultaneous Determination of
Amitriptyline Hydrochloride and Perphenazine,” J. Chem. Educ. 1998, 75, 1615–1618.
Goodney, D. E. “Analysis of Vitamin C by High-Pressure Liquid Chromatography,” J. Chem. Educ. 1987, 64, 187–188.
Guevremont, R.; Quigley, M. N. “Determination of Paralytic Shellfish Poisons Using Liquid Chromatography,” J. Chem. Educ.
1994, 71, 80–81.
Haddad, P.; Hutchins, S.; Tuffy, M. “High Performance Liquid Chromatography of Some Analgesic Compounds,” J. Chem.
Educ. 1983, 60, 166–168.
Huang, J.; Mabury, S. A.; Sagebiel, J. C. “Hot Chili Peppers: Extraction, Cleanup, and Measurement of Capscaicin,” J. Chem.
Educ. 2000, 77, 1630–1631.
Joeseph, S. M.; Palasota, J. A. “The Combined Effect of pH and Percent Methanol on the HPLC Separation of Benzoic Acid
and Phenol,” J. Chem. Educ. 2001, 78, 1381–1383.
Lehame, S. “The Separation of Copper, Iron, and Cobalt Tetramethylene Dithiocarbamates by HPLC,” J. Chem. Educ. 1986,
63, 727–728.
Luo, P.; Luo, M. Z.; Baldwin, R. P. “Determination of Sugars in Food Products,” J. Chem. Educ. 1993, 70, 679–681.
Mueller, B. L.; Potts, L. W. “HPLC Analysis of an Asthma Medication,” J. Chem. Educ. 1988, 65, 905–906.
Munari, M.; Miurin, M.; Goi, G. “Didactic Application to Riboflavin HPLC Analysis,” J. Chem. Educ. 1991, 68, 78–79.
Orth, D. L. “HPLC Determination of Taurine in Sports Drinks,” J. Chem. Educ. 2001, 78, 791–792.
Remcho, V. T.; McNair, H. M.; Rasmussen, H. T. “HPLC Method Development with the Photodiode Array Detector,” J. Chem.
Educ. 1992, 69, A117–A119.
Richardson, W. W., III; Burns, L. “HPLC of the Polypeptides in a Hydrolyzate of Egg-White Lysozyme,” J. Chem. Educ. 1988,
65, 162–163.
Silveira, A., Jr.; Koehler, J. A.; Beadel, E. F., Jr.; Monore, P. A. “HPLC Analysis of Chlorophyll a, Chlorophyll b, and βCarotene in Collard Greens,” J. Chem. Educ. 1984, 61, 264–265.
Siturmorang, M.; Lee, M. T. B.; Witzeman, L. K.; Heineman, W. R. “Liquid Chromatography with Electrochemical Detection
(LC-EC): An Experiment Using 4-Aminophenol,” J. Chem. Educ. 1998, 75, 1035–1038.
Sottofattori, E.; Raggio, R.; Bruno, O. “Milk as a Drug Analysis Medium: HPLC Determination of Isoniazid,” J. Chem. Educ.
2003, 80, 547–549.
Strohl, A. N. “A Study of Colas: An HPLC Experiment,” J. Chem. Educ. 1985, 62, 447–448.
Tran, C. D.; Dotlich, M. “Enantiomeric Separation of Beta-Blockers by High Performance Liquid Chromatography,” J. Chem.
Educ. 1995, 72, 71–73.
Van Arman, S. A.; Thomsen, M. W. “HPLC for Undergraduate Introductory Laboratories,” J. Chem. Educ. 1997, 74, 49–50.
Wingen, L. M.; Low, J. C.; Finlayson-Pitts, B. J. “Chromatography, Absorption, and Fluorescence: A New Instrumental
Analysis Experiment on the Measurement of Polycyclic Aromatic Hydrocarbons in Cigarette Smoke,” J. Chem. Educ. 1998, 75,
1599–1603.
Ion-Exchange Chromatography
Bello, M. A.; Gustavo González, A. “Determination of Phosphate in Cola Beverages Using Nonsuppressed Ion
Chromatography,” J. Chem. Educ. 1996, 73, 1174–1176.
Kieber, R. J.; Jones, S. B. “An Undergraduate Laboratory for the Determination of Sodium, Potassium, and Chloride,” J. Chem.
Educ. 1994, 71, A218–A222.
Koubek, E.; Stewart, A. E. “The Analysis of Sulfur in Coal,” J. Chem. Educ. 1992, 69, A146–A148.
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Sinniah, K.; Piers, K. “Ion Chromatography: Analysis of Ions in Pond Water,” J. Chem. Educ. 2001, 78, 358–362.
Xia, K.; Pierzynski, G. “Competitive Sorption between Oxalate and Phosphate in Soil: An Environmental Chemistry
Laboratory Using Ion Chromatography,” J. Chem. Educ. 2003, 80, 71–75.
Size-Exchange Chromatography
Brunauer, L. S.; Davis, K. K. “Size Exclusion Chromatography: An Experiment for High School and Community College
Chemistry and Biotechnology Laboratory Programs,” J. Chem. Educ. 2008, 85, 683–685.
Saiz, E.; Tarazona, M. P. “Size-Exclusion Chromatography Using Dual Detection,” Chem. Educator 2000, 5, 324–328.
Electrophoresis
Almarez, R. T.; Kochis, M. “Microscale Capillary Electrophoresis: A Complete Instrumentation Experiment for Chemistry
Students at the Undergraduate Junior or Senior Level,” J. Chem. Educ. 2003, 80, 316–319.
Beckers, J. L. “The Determination of Caffeine in Coffee: Sense or Nonsense?” J. Chem. Educ. 2004, 81, 90–93.
Beckers, J. L. “The Determination of Vanillin in a Vanilla Extract,” J. Chem. Educ. 2005, 82, 604–606.
Boyce, M. “Separation and Quantification of Simple Ions by Capillary Zone Electrophoresis,” J. Chem. Educ. 1999, 76, 815–
819.
Conradi, S.; Vogt, C.; Rohde, E. “Separation of Enatiomeric Barbiturates by Capillary Electrophoresis Using a CyclodextrinContaining Run Buffer,” J. Chem. Educ. 1997, 74, 1122–1125.
Conte, E. D.; Barry, E. F.; Rubinstein, H. “Determination of Caffeine in Beverages by Capillary Zone Electrophoresis,” J.
Chem. Educ. 1996, 73, 1169–1170.
Demay, S.; Martin-Girardeau, A.; Gonnord, M.-F. “Capillary Electrophoretic Quantitative Analysis of Anions in Drinking
Water,” J. Chem. Educ. 1999, 76, 812–815.
Emry, R.; Cutright, R. D.; Wright, J.; Markwell, J. “Candies to Dye for: Cooperative, Open-Ended Student Activities to
Promote Understanding of Electrophoretic Fractionation,” J. Chem. Educ. 2000, 77, 1323–1324.
Gardner, W. P.; Girard, J. E. “Analysis of Common Household Cleaner-Disinfectants by Capillary Electrophoresis,” J. Chem.
Educ. 2000, 77, 1335–1338.
Gruenhagen, J. A.; Delaware, D.; Ma, Y. “Quantitative Analysis of Non-UV-Absorbing Cations in Soil Samples by HighPerformance Capillary Electrophoresis,” J. Chem. Educ. 2000, 77, 1613–1616.
Hage, D. S.; Chattopadhyay, A.; Wolfe, C. A. C.; Grundman, J.; Kelter, P. B. “Determination of Nitrate and Nitrite in Water by
Capillary Electrophoresis,” J. Chem. Educ. 1998, 75, 1588–1590.
Herman, H. B.; Jezorek, J. R.; Tang, Z. “Analysis of Diet Tonic Water Using Capillary Electrophoresis,” J. Chem. Educ. 2000,
77, 743–744.
Janusa, M. A.; Andermann, L. J.; Kliebert, N. M.; Nannie, M. H. “Determination of Chloride Concentration Using Capillary
Electrophoresis,” J. Chem. Educ. 1998, 75, 1463–1465.
McDevitt, V. L.; Rodríguez, A.; Williams, K. R. “Analysis of Soft Drinks: UV Spectrophotometry, Liquid Chromatography, and
Capillary Electrophoresis,” J. Chem. Educ. 1998, 75, 625–629.
Palmer, C. P. “Demonstrating Chemical and Analytical Concepts in the Undergraduate Laboratory Using Capillary
Electrophoresis and Micellar Electrokinetic Chromatography,” J. Chem. Educ. 1999, 76, 1542–1543.
Pursell, C. J.; Chandler, B.; Bushey, M. M. “Capillary Electrophoresis Analysis of Cations in Water Samples,” J. Chem. Educ.
2004, 81, 1783–1786.
Solow, M. “Weak Acid pKa Determination Using Capillary Zone Electrophoresis,” J. Chem. Educ. 2006, 83, 1194–1195.
Thompson, L.; Veening, H.; Strain, T. G. “Capillary Electrophoresis in the Undergraduate Instrumental Analysis Laboratory:
Determination of Common Analgesic Formulations,” J. Chem. Educ. 1997, 74, 1117–1121.
Vogt, C.; Conradi, S.; Rhode, E. “Determination of Caffeine and Other Purine Compounds in Food and Pharmaceuticals by
Micellar Electrokinetic Chromatography” J. Chem. Educ. 1997, 74, 1126–1130.
Weber, P. L.; Buck, D. R. “Capillary Electrophoresis: A Fast and Simple Method for the Determination of the Amino Acid
Composition of Proteins,” J. Chem. Educ. 1994, 71, 609–612.
Welder, F.; Colyer, C. L. “Using Capillary Electrophoresis to Determine the Purity of Acetylsalicylic Acid Synthesized in the
Undergraduate Laboratory,” J. Chem. Educ. 2001, 78, 1525–1527.
Williams, K. R.; Adhyaru, B.; German, I.; Russell, T. “Determination of a Diffusion Coefficient by Capillary Electrophoresis,”
J. Chem. Educ. 2002, 79, 1475–1476.
The following texts provide a good introduction to the broad field of separations, including chromatography and electrophoresis.
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Giddings, J. C. Unified Separation Science, Wiley-Interscience: New York 1991.
Karger, B. L.; Snyder, L. R.; Harvath, C. An Introduction to Separation Science, Wiley-Interscience: New York, 1973
Miller, J. M. Separation Methods in Chemical Analysis, Wiley-Interscience: New York, 1975.
Poole, C. F. The Essence of Chromatography, Elsevier: Amsterdam, 2003.
A more recent discussion of peak capacity is presented in the following paper.
Davis, J. M.; Stoll, D. R.; Carr, P. W. “Dependence of Effective Peak Capacity in Comprehensive Two-Dimensional Separations
on the Distribution of Peak Capacity between the Two Dimensions,” Anal. Chem. 2008, 80, 8122–8134.
Li, X.; Stoll, D. R.; Carr, P. W. “Equation for Peak Capacity Estimation in Two-Dimensional Liquid Chromatography,” Anal.
Chem. 2009, 81, 845–850.
Shen, Y.; Lee, M. “General Equation for Peak Capacity in Column Chromatography,” Anal. Chem. 1998, 70, 3853–3856.
The following references may be consulted for more information on gas chromatography.
Grob, R. L., ed, Modern Practice of Gas Chromatography, Wiley-Interscience: New York, 1972.
Hinshaw, J. V. “A Compendium of GC Terms and Techniques,” LC•GC 1992, 10, 516–522.
Ioffe, B. V.; Vitenberg, A. G. Head-Space Analysis and Related Methods in Gas Chromatography, Wiley-Interscience: New
York, 1982.
Kitson, F. G.; Larsen, B. S.; McEwen, C. N. Gas Chromatography and Mass Spectrometry: A Practical Guide, Academic Press:
San Diego, 1996.
McMaster, M. C. GC/MS: A Practical User’s Guide, Wiley-Interscience: Hoboken, NJ, 2008.
The following references provide more information on high-performance liquid chromatography.
Dorschel, C. A.; Ekmanis, J. L.; Oberholtzer, J. E.; Warren, Jr. F. V.; Bidlingmeyer, B. A. “LC Detectors,” Anal. Chem. 1989,
61, 951A–968A.
Ehlert, S.; Tallarek, U. “High-pressure liquid chromatography in lab-on-a-chip devices,” Anal. Bioanal. Chem. 2007, 388, 517–
520.
Francois, I.; Sandra, K.; Sandra, P. “Comprehensive liquid chromatography: Fundamental aspects and practical considerations
—A review,” Anal. Chim. Acta 2009, 641, 14–31.
Harris, C. M. “Shrinking the LC Landscape,” Anal. Chem. 2003, 75, 64A–69A.
Meyer, V. R. Pitfalls and Errors of HPLC in Pictures, Wiley-VCH: Weinheim, Germany, 2006.
Pozo, O. J.; Van Eenoo, P.; Deventer, K.; Delbeke, F. T. “Detection and characterization of anabolic steroids in doping analysis
by LC–MS,” Trends Anal. Chem. 2008, 27, 657–671.
Scott, R. P. W. “Modern Liquid Chromatography,” Chem. Soc. Rev. 1992, 21, 137–145.
Simpson, C. F., ed. Techniques in Liquid Chromatography, Wiley-Hayden: Chichester, England; 1982.
Snyder, L. R.; Glajch, J. L.; Kirkland, J. J. Practical HPLC Method Development, Wiley-Interscience: New York,1988.
van de Merbel, N. C. “Quantitative determination of endogenous compounds in biological samples using chromatographic
techniques,” Trends Anal. Chem. 2008, 27, 924–933.
Yeung, E. S. “Chromatographic Detectors: Current Status and Future Prospects,” LC•GC 1989, 7, 118–128.
The following references may be consulted for more information on ion chromatography.
Shpigun, O. A.; Zolotov, Y. A. Ion Chromatography in Water Analysis, Ellis Horwood: Chichester, England, 1988.
Smith, F. C. Jr.; Chang, R. C. The Practice of Ion Chromatography, Wiley-Interscience: New York, 1983.
The following references may be consulted for more information on supercritical fluid chromatography.
Palmieri, M. D. “An Introduction to Supercritical Fluid Chromatography. Part I: Principles and Applications,” J. Chem. Educ.
1988, 65, A254–A259.
Palmieri, M. D. “An Introduction to Supercritical Fluid Chromatography. Part II: Applications and Future Trends,” J. Chem.
Educ. 1989, 66, A141–A147.
The following references may be consulted for more information on capillary electrophoresis.
Baker, D. R. Capillary Electrophoresis, Wiley-Interscience: New York, 1995.
Copper, C. L. “Capillary Electrophoresis: Part I. Theoretical and Experimental Background,” J. Chem. Educ. 1998, 75, 343–
347.
Copper, C. L.; Whitaker, K. W. “Capillary Electrophoresis: Part II. Applications,” J. Chem. Educ. 1998, 75, 347–351.
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DeFrancesco, L. “Capillary Electrophoresis: Finding a Niche,” Today’s Chemist at Work, February 2002, 59–64.
Ekins, R. P. “Immunoassay, DNA Analysis, and Other Ligand Binding Assay Techniques: From Electropherograms to
Multiplexed, Ultrasensative Microarrays on a Chip,” J. Chem. Educ. 1999, 76, 769–780.
Revermann, T.; Götz, S.; Künnemeyer, J.; Karst, U. “Quantitative analysis by microchip capillary electrophoresis—current
limitations and problem-solving strategies,” Analyst 2008, 133, 167–174.
Timerbaev, A. R. “Capillary electrophoresis coupled to mass spectrometry for biospeciation analysis: critical evaluation,”
Trends Anal. Chem. 2009, 28, 416–425.
Unger, K. K.; Huber, M.; Hennessy, T. P.; Hearn, M. T. W.; Walhagen, K. “A Critical Appraisal of Capillary
Electrochromatography,” Anal. Chem. 2002, 74, 200A–207A.
Varenne, A.; Descroix, S. “Recent strategies to improve resolution in capillary electrophoresis—A review,” Anal. Chim. Acta
2008, 628, 9–23.
Vetter, A. J.; McGowan, G. J. “The Escalator—An Analogy for Explaining Electroosmotic Flow,” J. Chem. Educ. 2001, 78,
209–211.
Xu, Y. “Tutorial: Capillary Electrophoresis,” Chem. Educator, 1996, 1(2), 1–14.
The application of spreadsheets and computer programs for modeling chromatography is described in the following papers.
Abbay, G. N.; Barry, E. F.; Leepipatpiboon, S.; Ramstad, T.; Roman, M. C.; Siergiej, R. W.; Snyder, L. R.; Winniford, W. L.
“Practical Applications of Computer Simulation for Gas Chromatography Method Development,” LC•GC 1991, 9, 100–114.
Drouen, A.; Dolan, J. W.; Snyder, L. R.; Poile, A.; Schoenmakers, P. J. “Software for Chromatographic Method Development,”
LC•GC 1991, 9, 714–724.
Kevra, S. A.; Bergman, D. L.; Maloy, J. T. “A Computational Introduction to Chromatographic Bandshape Analysis,” J. Chem.
Educ. 1994, 71, 1023–1028.
Rittenhouse, R. C. “HPLC for Windows: A Computer Simulation of High-Performance Liquid Chromatography,” J. Chem.
Educ. 1995, 72, 1086–1087.
Shalliker, R. A.; Kayillo, S.; Dennis, G. R. “Optimizing Chromatographic Separations: An Experiment Using an HPLC
Simulator,” J. Chem. Educ. 2008, 85, 1265–1268.
Sundheim, B. R. “Column Operations: A Spreadsheet Model,” J. Chem. Educ. 1992, 69, 1003–1005.
The following papers discuss column efficiency, peak shapes, and overlapping chromatographic peaks.
Bildingmeyer, B. A.; Warren, F. V., Jr. “Column Efficiency Measurement,” Anal. Chem. 1984, 56, 1583A–1596A.
Hawkes, S. J. “Distorted Chromatographic Peaks,” J. Chem. Educ. 1994, 71, 1032–1033.
Hinshaw, J. “Pinning Down Tailing Peaks,” LC•GC 1992, 10, 516–522.
Meyer, V. K. “Chromatographic Integration Errors: A Closer Look at a Small Peak,” LC•GC North America 2009, 27, 232–
244.
Reid, V. R.; Synovec, R. E. “High-speed gas chromatography: The importance of instrumentation optimization and the
elimination of extra-column band broadening,” Talanta2008, 76, 703–717.
Chapter 13
The following set of experiments introduce students to the applications of chemical kinetic methods, including enzyme kinetic
methods, and flow injection analysis.
Chemical Kinetic Methods
Abramovitch, D. A.; Cunningham, L. K.; Litwer, M. R. “Decomposition Kinetics of Hydrogen Perox- ide: Novel Lab
Experiments Employing Computer Technology,” J. Chem. Educ. 2003, 80, 790–792.
Bateman, Jr. R. C.; Evans, J. A. “Using the Glucose Oxidase/Peroxidase Systems in Enzyme Kinetics,” J. Chem. Educ. 1995,
72, A240–A241.
Bendinskas, K.; DiJacomo, C.; Krill, A.; Vitz, E. “Kinetics of Alcohol Dehydrogenase-Catalyzed Oxidation of Ethanol
Followed by Visible Spectroscopy,” J. Chem. Educ. 1068, 82, 1068–1070.
Clark, C. R. “A Stopped-Flow Kinetics Experiment for Advanced Undergraduate Laboratories: Formation of Iron(III)
Thiocyanate,” J. Chem. Educ. 1997, 74, 1214–1217.
Diamandis, E. P.; Koupparis, M. A.; Hadjiionnou, T. P. “Kinetic Studies with Ion-Selective Electrodes: Determination of
Creatinine in Urine with a Picrate Ion-Selective Electrode,” J. Chem. Educ. 1983, 60, 74–76.
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Frey, M. W.; Frey, S. T.; Soltau, S. R. “Exploring the pH Dependence of L-leucine-p-nitroanilide Cleavage by Aminopeptidase
Aeromonas Proteolytica: A Combined Buffer-Enzyme Kinetics Experiment for the General Chemistry Laboratory,” Chem.
Educator 2010, 15, 117-120.
Gooding, J. J.; Yang, W.; Situmorang, M. “Bioanalytical Experiments for the Undergraduate Laboratory: Monitoring Glucose
in Sport Drinks,” J. Chem. Educ. 2001, 78, 788–790.
Hamilton, T. M.; Dobie-Galuska, A. A.; Wietstock, S. M. “The o-Phenylenediamine-Horseradish Peroxidase System: Enzyme
Kinetics in the General Chemistry Lab,” J. Chem. Educ. 1999, 76, 642– 644.
Johnson, K. A. “Factors Affecting Reaction Kinetics of Glucose Oxidase,” J. Chem. Educ. 2002, 79,74–76.
Mowry, S.; Ogren, P. J. “Kinetics of Methylene Blue Reduction by Ascorbic Acid,” J. Chem. Educ. 1999, 76, 970–974.
Nyasulu, F. W.; Barlag, R. “Gas Pressure Sensor Monitored Iodide-Catalyzed Decomposition Kinetics of Hydrogen Peroxide:
An Initial Rate Approach,” Chem. Educator 2008, 13, 227–230.
Nyasulu, F. W.; Barlag, R. “Thermokinetics: Iodide-Catalyzed Decomposition Kinetics of Hydrogen Peroxide; An Integrated
Rate Approach,” Chem. Educator 2010, 15, 168–170.
Pandey, S.; McHale, M. E. R.; Horton, A. M.; Padilla, S. A.; Trufant, A. L.; De La Sancha, N. U.; Vela, E.; Acree, Jr., W. E.
“Kinetics-Based Indirect Spectrophotometric Method for the Simultaneous Determination of MnO4–and Cr2O72–,” J. Chem.
Educ. 1998, 75, 450–452.
Stock, E.; Morgan, M. “A Spectroscopic Analysis of the Kinetics of the Iodine Clock Reaction without Starch,” Chem.
Educator 2010, 15, 158–161.
Vasilarou, A.-M. G.; Georgiou, C. A. “Enzymatic Spectrophotometric Reaction Rate Determination of Glucose in Fruit Drinks
and Carbonated Beverages,” J. Chem. Educ. 2000, 77, 1327–1329.
Williams, K. R.; Adhyaru, B.; Timofeev, J.; Blankenship, M. K. “Decomposition of Aspartame. A Kinetics Experiment for
Upper-Level Chemistry Laboratories,” J. Chem. Educ. 2005, 82, 924–925.
Flow Injection Methods
Carroll, M. K.; Tyson, J. F. “An Experiment Using Time-Based Detection in Flow Injection Analysis,” J. Chem. Educ. 1993,
70, A210–A216.
Conceição, A. C. L.; Minas da Piedade, M. E. “Determination of Acidity Constants by Gradient Flow-Injection Titration,” J.
Chem. Educ. 2006, 83, 1853–1856.
Hansen, E. H.; Ruzicka, J. “The Principles of Flow Injection Analysis as Demonstrated by Three Lab Exercises,” J. Chem.
Educ. 1979, 56, 677–680.
McKelvie, I. D.; Cardwell, T. J.; Cattrall, R. W. “A Microconduit Flow Injection Analysis Demonstration using a 35-mm Slide
Projector,” J. Chem. Educ. 1990, 67, 262–263.
Meyerhoff, M. E.; Kovach, P. M. “An Ion-Selective Electrode/Flow Injection Analysis Experiment: Determination of Potassium
in Serum,” J. Chem. Educ. 1983, 60, 766–768.
Nóbrega, J. A.; Rocha, F. R. P. “Ionic Strength Effect on the Rate of Reduction of Hexacyanoferrate(II) by Ascorbic Acid,” J.
Chem. Educ. 1997, 74, 560–562.
Ríos, A.; Luque de Castro, M.; Valcárcel, M. “Determination of Reaction Stoichiometries by Flow Injection Analysis,” J.
Chem. Educ. 1986, 63, 552–553.
Stults, C. L. M.; Wade, A. P.; Crouch, S. R. “Investigation of Temperature Effects on Dispersion in a Flow Injection Analyzer,”
J. Chem. Educ. 1988, 65, 645–647.
Wolfe, C. A. C.; Oates, M. R.; Hage, D. S. “Automated Protein Assay Using Flow Injection Analysis,” J. Chem. Educ. 1998,
75, 1025–1028.
The following sources provides a general review of the importance of chemical kinetics in analytical chemistry.
Bergmyer, H. U.; Grassl, M. Methods of Enzymatic Analysis, Verlag Chemie: Deerfield Beach, FL, 3rd Ed., 1983.
Laitinen, H. A.; Ewing, G. W., eds., A History of Analytical Chemistry, The Division of Analytical Chemistry of the American
Chemical Society: Washington, D. C., 1977, pp. 97–102.
Malmstadt, H. V.; Delaney, C. J.; Cordos, E. A. “Reaction-Rate Methods of Chemical Analysis,” Crit. Rev. Anal. Chem. 1972,
2, 559–619.
Mark, H. B.; Rechnitz, G. A. Kinetics in Analytical Chemistry, Wiley: New York, 1968.
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Mottola, H. A. “Catalytic and Differential Reaction-Rate Methods of Chemical Analysis,” Crit. Rev. Anal. Chem. 1974, 4, 229–
280.
Mottola, H. A. “Some Kinetic Aspects Relevant to Contemporary Analytical Chemistry,” J. Chem. Educ. 1981, 58, 399–403.
Mottola, H. A. Kinetic Aspects of Analytical Chemistry, Wiley: New York, 1988.
Pardue, H. L. “A Comprehensive Classification of Kinetic Methods of Analysis Used in Clinical Chemistry,” Clin. Chem. 1977,
23, 2189–2201.
Pardue, H. L. “Kinetic Aspects of Analytical Chemistry,” Anal. Chim. Acta, 1989, 216, 69–107.
Perez-Bendito, D.; Silva, M. Kinetic Methods in Analytical Chemistry, Ellis Horwood: Chichester, 1988.
Pisakiewicz, D. Kinetics of Chemical and Enzyme-Catalyzed Reactions, Oxford University Press: New York, 1977.
The following instrumental analysis textbooks may be consulted for further information on the detectors and signal analyzers used
in radiochemical methods of analysis.
Skoog, D. A.; Holler, F. J.; Nieman, T. A. Principles of Instrumental Analysis, 5th Ed., Saunders College Publishing/Harcourt
Brace and Co.: Philadelphia., 1998, Chapter 32.
Strobel, H. A.; Heineman, W. R. Chemical Instrumentation: A Systematic Approach, 3rd Ed., Wiley-Interscience: New York,
1989.
The following resources provide additional information on the theory and application of flow injection analysis.
Andrew, K. N.; Blundell, N. J.; Price, D.; Worsfold, P. J. “Flow Injection Techniques for Water Monitoring,” Anal. Chem. 1994,
66, 916A–922A.
Betteridge, D. “Flow Injection Analysis,” Anal. Chem. 1978, 50, 832A–846A.
Kowalski, B. R.; Ruzicka, J. Christian, G. D. “Flow Chemography - The Future of Chemical Education,” Trends Anal. Chem.
1990, 9, 8–13.
Mottola, H. A. “Continuous Flow Analysis Revisited,” Anal. Chem. 1981, 53, 1312A–1316A.
Ruzicka, J. “Flow Injection Analysis: From Test Tube to Integrated Microconduits,” Anal. Chem. 1983, 55, 1040A–1053A.
Ruzicka, J.; Hansen, E. H. Flow-Injection Analysis, Wiley-Interscience: New York, 1989.
Ruzicka, J.; Hansen, E. H. “Retro-Review of Flow-Injection Analysis,” Trends Anal. Chem. 2008, 27,390–393.
Silvestre, C. I. C.; Santos, J. L. M.; Lima, J. L. F. C.; Zagatto, E. A. G. “Liquid-Liquid Extraction in Flow Analysis: A Critical
Review,” Anal. Chim. Acta 2009, 652, 54–65.
Stewart, K. K. “Flow Injection Analysis: New Tools for Old Assays, New Approaches to Analytical Measurements,” Anal.
Chem. 1983, 55, 931A–940A.
Tyson, J. F. “Atomic Spectrometry and Flow Injection Analysis: A Synergic Combination,” Anal. Chim. Acta, 1988, 214, 57–
75.
Valcarcel, M.; Luque de Castro, M. D. Flow-Injection Analysis: Principles and Applications, Ellis Horwood: Chichester,
England, 1987.
Chapter 14
The following set of experiments provide practical examples of the optimization of experimental conditions. Examples include
simplex optimization, factorial designs for developing empirical models of response surfaces, and fitting experimental data to
theoretical models of the response surface.
Amenta, D. S.; Lamb, C. E.; Leary, J. J. “Simplex Optimization of Yield of sec-Butylbenzene in a Friedel-Crafts Alkylation,” J.
Chem. Educ. 1979, 56, 557–558.
Harvey, D. T.; Byerly, S.; Bowman, A.; Tomlin, J. “Optimization of HPLC and GC Separations Using Response Surfaces,” J.
Chem. Educ. 1991, 68, 162–168.
Leggett, D. L. “Instrumental Simplex Optimization,” J. Chem. Educ. 1983, 60, 707–710.
Oles, P. J. “Fractional Factorial Experimental Design as a Teaching Tool for Quantitative Analysis,” J. Chem. Educ. 1998, 75,
357–359.
Palasota, J. A.; Deming, S.N. “Central Composite Experimental Design,” J. Chem. Educ. 1992, 69, 560–561.
Sangsila, S.; Labinaz, G.; Poland, J. S.; vanLoon, G. W. “An Experiment on Sequential Simplex Optimization of an Atomic
Absorption Analysis Procedure,” J. Chem. Educ. 1989, 66, 351–353.
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Santos-Delgado, M. J.; Larrea-Tarruella, L. “A Didactic Experience of Statistical Analysis for the Determination of Glycine in a
Nonaqueous Medium using ANOVA and a Computer Program,” J. Chem. Educ. 2004, 81, 97–99.
Shavers, C. L.; Parsons, M. L.; Deming, S. N. “Simplex Optimization of Chemical Systems,” J. Chem Educ. 1979, 56, 307–
309.
Stieg, S. “A Low-Noise Simplex Optimization Experiment,” J. Chem. Educ. 1986, 63, 547–548.
Stolzberg, R. J. “Screening and Sequential Experimentation: Simulations and Flame Atomic Absorption Spectrometry
Experiments,” J. Chem. Educ. 1997, 74, 216–220.
Van Ryswyk, H.; Van Hecke, G. R. “Attaining Optimal Conditions,” J. Chem. Educ. 1991, 66, 878–882.
The following texts and articles provide an excellent discussion of optimization methods based on searching algorithms and
mathematical modeling use factorial designs, including a discussion of the relevant calculations. A few of these sources discuss
other types of experimental designs.
Bayne, C. K.; Rubin, I. B. Practical Experimental Designs and Optimization Methods for Chemists, VCH Publishers: Deerfield
Beach, FL; 1986.
Box, G. E. P. “Statistical Design in the Study of Analytical Methods,” Analyst 1952, 77, 879–891.
Deming, S. N.; Morgan, S. L. Experimental Design: A Chemometric Approach, Elsevier: Amsterdam, 1987.
Ferreira, S. L. C.; dos Santos, W. N. L.; Quintella, C. M.; Neto, B. B.; Bosque-Sendra, J. M. “Doehlert • Matrix: A
Chemometric Tool for Analytical Chemistry—Review,” Talanta 2004, 63, 1061–1067.
Ferreira, S. L. C.; Bruns, R. E.; Ferreira, H. S.; Matos, G. D.; David, J. M.; Brandão, G. C.; da Silva, E. G. P.; Portugal, L. A.;
dos Reis, P. S.; Souza, A. S.; dos Santos, W. N. L. “Box-Behnken Design: An Alternative for the Optimization of Analytical
Methods,” Anal. Chim. Acta 2007, 597, 179–186.
Gonzalez, A. G. “Two Level Factorial Experimental Designs Based on Multiple Linear Regression Models: A Tutorial Digest
Illustrated by Case Studies,” Anal. Chim. Acta 1998, 360, 227–241.
Goupy, J. “What Kind of Experimental Design for Finding and Checking Robustness of Analytical Methods?” Anal. Chim. Acta
2005, 544, 184–190.
Hendrix, C. D. “What Every Technologist Should Know About Experimental Design,” Chemtech 1979, 9, 167–174.
Hendrix, C. D. “Through the Response Surface with Test Tube and Pipe Wrench,” Chemtech 1980, 10, 488–497.
Leardi, R. “Experimental Design: A Tutorial,” Anal. Chim. Acta 2009, 652, 161–172.
Liang, Y. “Comparison of Optimization Methods,” Chromatography Review 1985, 12(2), 6–9.
Morgan, E. Chemometrics: Experimental Design, John Wiley and Sons: Chichester, 1991.
Thompson, M., ed. “Experimental Design and Optimization (1): An Introduction to Some Basic Concepts,” AMC Technical
Brief 24, June 2006.
Thompson, M., ed. “Experimental Design and Optimization (2): Handling Uncontrolled Factors” AMC Technical Brief 26,
December 2006.
Thompson, M., ed. “Experimental Design and Optimization (3): Some Fractional Factorial Designs,” AMC Technical Brief 36,
January 2009.
Walters, F. H.; Morgan, S. L.; Parker, L. P., Jr.; Deming, S. N. Sequential Simplex Optimization, CRC Press: Boca Raton, FL,
1991. (an electronic version of this text is freely available from Multisimplex AB and is available here.)
The following texts provide additional information about ANOVA calculations, including discussions of two-way analysis of
variance.
Graham, R. C. Data Analysis for the Chemical Sciences, VCH Publishers: New York, 1993.
Miller, J. C.; Miller, J. N. Statistics for Analytical Chemistry, Ellis Horwood Limited: Chichester, 1988.
The following resources provide additional information on the validation of analytical methods.
Gonzalez, A. G.; Herrador, M. A. “A Practical Guide to Analytical Method Validation, Including Measurement Uncertainty and
Accuracy Profiles,” Trends Anal. Chem. 2007, 26, 227–238.
Thompson, M.; Ellison, S. L. R.; Wood, R. “Harmonized Guidelines for Single-Laboratory Validation of Analytical Methods,”
Pure Appl. Chem. 2002, 74, 835–855.
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Chapter 15
The following three experiments introduce aspects of quality assurance and quality control.
Bell, S. C.; Moore, J. “Integration of Quality Assurance/Quality Control into Quantitative Analysis,” J. Chem. Educ. 1998, 75,
874–877.
Cancilla, D. A. “Integration of Environmental Analytical Chemistry with Environmental Law: The Development of a ProblemBased Laboratory,” J. Chem. Educ. 2001, 78, 1652–1660.
Laquer, F. C. “Quality Control Charts in the Quantitative Analysis Laboratory Using Conductance Measurement,” J. Chem.
Educ. 1990, 67, 900–902.
Marcos, J.; Ríos, A.; Valcárcel, M. “Practicing Quality Control in a Bioanalytical Experiment,” J. Chem. Educ. 1995, 72, 947–
949.
The following texts and articles may be consulted for an additional discussion of quality assurance and quality control.
Amore, F. “Good Analytical Practices,” Anal. Chem. 1979, 51, 1105A–1110A.
Barnard, Jr. A. J.; Mitchell, R. M.; Wolf, G. E. “Good Analytical Practices in Quality Control,” Anal. Chem. 1978, 50, 1079A–
1086A.
Cairns, T.; Rogers, W. M. “Acceptable Analytical Data for Trace Analysis,” Anal. Chem. 1993, 55, 54A–57A.
Taylor, J. K. Quality Assurance of Chemical Measurements, Lewis Publishers: Chelsa, MI, 1987.
Additional information about the construction and use of control charts may be found in the following sources.
Miller, J. C.; Miller, J. N. Statistics for Analytical Chemistry, 2nd Ed., Ellis Horwood Limited: Chichester, 1988.
Ouchi, G. I. “Creating Control Charts with a Spreadsheet Program,” LC•GC 1993, 11, 416–423.
Ouchi, G. I. “Creating Control Charts with a Spreadsheet Program,” LC•GC 1997, 15, 336–344.
Simpson, J. M. “Spreadsheet Statistics,” J. Chem. Educ. 1994, 71, A88–A89.
Contributors
David Harvey (DePauw University)
This page titled 17: Additional Resources is shared under a CC BY-NC-SA 4.0 license and was authored, remixed, and/or curated by David
Harvey.
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CHAPTER OVERVIEW
18: Back Matter
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Front Matter
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Table of Contents
Analytical chemistry spans nearly all areas of chemistry but involves the development of tools and methods to measure physical
properties of substances and apply those techniques to the identification of their presence (qualitative analysis) and quantify the
amount present (quantitative analysis) of species in a wide variety of settings.
1: Front Matter
1.1: TitlePage
1.2: InfoPage
1.3: Table of Contents
2: Introduction to Analytical Chemistry
2.1: What is Analytical Chemistry?
2.2: The Analytical Perspective
2.3: Common Analytical Problems
2.4: Introduction to Analytical Chemistry (Exercises)
2.5: Introduction to Analytical Chemistry (Summary)
3: Basic Tools of Analytical Chemistry
In the chapters that follow we will explore many aspects of analytical chemistry. In the process we will consider important
questions such as “How do we treat experimental data?”, “How do we ensure that our results are accurate?”, “How do we
obtain a representative sample?”, and “How do we select an appropriate analytical technique?” Before we look more closely at
these and other questions, we will first review some basic tools of importance to analytical chemists.
3.1: Measurements in Analytical Chemistry
3.2: Concentration
3.3: Stoichiometric Calculations
3.4: Basic Equipment
3.5: Preparing Solutions
3.6: Spreadsheets and Computational Software
3.7: The Laboratory Notebook
3.8: Basic Tools of Analytical Chemistry (Exercises)
3.9: Basic Tools of Analytical Chemistry (Summary)
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4: The Vocabulary of Analytical Chemistry
If you leaf through an issue of the journal Analytical Chemistry, you will soon discover that the authors and readers share a
common vocabulary of analytical terms. You are probably familiar with some of these terms, such as accuracy and precision,
but other terms, such as analyte and matrix may be less familiar to you. In order to participate in the community of analytical
chemists, you must first understand its vocabulary.
4.1: Analysis, Determination, and Measurement
4.2: Techniques, Methods, Procedures, and Protocols
4.3: Classifying Analytical Techniques
4.4: Selecting an Analytical Method
4.5: Developing the Procedure
4.6: Protocols
4.7: The Importance of Analytical Methodology
4.8: The Vocabulary of Analytical Chemistry (Exercises)
4.9: The Vocabulary of Analytical Chemistry (Summary)
5: Evaluating Analytical Data
When using an analytical method we make three separate evaluations of experimental error. First, before beginning an analysis
we evaluate potential sources of errors to ensure that they will not adversely effect our results. Second, during the analysis we
monitor our measurements to ensure that errors remain acceptable. Finally, at the end of the analysis we evaluate the quality of
the measurements and results, comparing them to our original design criteria.
5.1: Characterizing Measurements and Results
5.2: Characterizing Experimental Errors
5.3: Propagation of Uncertainty
5.4: The Distribution of Measurements and Results
5.5: Statistical Analysis of Data
5.6: Statistical Methods for Normal Distributions
5.7: Detection Limits
5.8: Using Excel and R to Analyze Data
5.9: Evaluating Analytical Data (Exercises)
5.10: Evaluating Analytical Data (Summary)
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6: Standardizing Analytical Methods
Standardization is the process of determining the relationship between the signal and the amount of analyte in a sample.
Previously, we defined this relationship as Stotal=kACA+Sreag where Stotal is the signal, nA is the moles of analyte, CA is the
analyte’s concentration, kA is the method’s sensitivity for the analyte, and Sreag is the contribution to Stotal from sources other
than the sample. To standardize a method we must determine values for kA and Sreag, which is the subject of this chapt
6.1: Analytical Standards
6.2: Calibrating the Signal
6.3: Determining the Sensitivity
6.4: Linear Regression and Calibration Curves
6.5: Blank Corrections
6.6: Using Excel and R for a Regression Analysis
6.7: Standardizing Analytical Methods (Exercises)
6.8: Standardizing Analytical Methods (Summary)
7: Equilibrium Chemistry
Regardless of the problem on which an analytical chemist is working, its solution requires a knowledge of chemistry and the
ability to apply that knowledge. For example, an analytical chemist studying the effect of pollution on spruce trees needs to
know the chemical differences between p‑hydroxybenzoic acid and p‑hydroxyacetophenone, two phenols found in the needles
of spruce trees. Your ability to “think as a chemist” is a product of your experience in the classroom and in the laboratory.
7.1: Reversible Reactions and Chemical Equilibria
7.2: Thermodynamics and Equilibrium Chemistry
7.3: Manipulating Equilibrium Constants
7.4: Equilibrium Constants for Chemical Reactions
7.5: Le Châtelier’s Principle
7.6: Ladder Diagrams
7.7: Solving Equilibrium Problems
7.8: Buffer Solutions
7.9: Activity Effects
7.10: Using Excel and R to Solve Equilibrium Problems
7.11: Some Final Thoughts on Equilibrium Calculations
7.12: Equilibrium Chemistry (Exercises)
7.13: Equilibrium Chemistry (Summary)
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8: Collecting and Preparing Samples
When we use an analytical method to solve a problem, there is no guarantee that our results will be accurate or precise. In
designing an analytical method we consider potential sources of determinate error and indeterminate error, and take appropriate
steps to minimize their effect, such as including reagent blanks and calibrating instruments. Why might a carefully designed
analytical method give poor results? One possibility is that we may have failed to account for errors with the sample.
8.1: The Importance of Sampling
8.2: Designing a Sampling Plan
8.3: Implementing the Sampling Plan
8.4: Separating the Analyte from Interferents
8.5: General Theory of Separation Efficiency
8.6: Classifying Separation Techniques
8.7: Liquid–Liquid Extractions
8.8: Separation Versus Preconcentration
8.9: Collecting and Preparing Samples (Exercises)
8.10: Collecting and Preparing Samples (Summary)
9: Gravimetric Methods
Gravimetry includes all analytical methods in which the analytical signal is a measurement of mass or a change in mass. When
you step on a scale after exercising you are making, in a sense, a gravimetric determination of your mass. Mass is the most
fundamental of all analytical measurements, and gravimetry is unquestionably our oldest quantitative analytical technique.
9.1: Overview of Gravimetric Methods
9.2: Precipitation Gravimetry
9.3: Volatilization Gravimetry
9.4: Particulate Gravimetry
9.5: Gravimetric Methods (Exercises)
9.6: Gravimetric Methods (Summary)
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10: Titrimetric Methods
Titrimetry, in which volume serves as the analytical signal, made its first appearance as an analytical method in the early
eighteenth century. Titrimetric methods were not well received by the analytical chemists of that era because they could not
duplicate the accuracy and precision of a gravimetric analysis. Not surprisingly, few standard texts from the 1700s and 1800s
include titrimetric methods of analysis.
10.1: Overview of Titrimetry
10.2: Acid–Base Titrations
10.3: Complexation Titrations
10.4: Redox Titrations
10.5: Precipitation Titrations
10.6: Titrimetric Methods (Exercises)
10.7: Titrimetric Methods (Summary)
11: Spectroscopic Methods
"Colorimetry" is one example of a spectroscopic method of analysis. At the end of the nineteenth century, spectroscopy was
limited to the absorption, emission, and scattering of visible, ultraviolet, and infrared electromagnetic radiation. Since its
introduction, spectroscopy has expanded to include other forms of electromagnetic radiation—such as X-rays, microwaves, and
radio waves—and other energetic particles—such as electrons and ions.
11.1: Overview of Spectroscopy
11.2: Spectroscopy Based on Absorption
11.03: UV
11.3: UV/Vis and IR Spectroscopy
11.4: Atomic Absorption Spectroscopy
11.5: Emission Spectroscopy
11.6: Photoluminescence Spectroscopy
11.7: Atomic Emission Spectroscopy
11.8: Spectroscopy Based on Scattering
11.9: Spectroscopic Methods (Exercises)
11.10: Spectroscopic Methods (Summary)
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12: Electrochemical Methods
In Chapter 10 we examined several spectroscopic techniques that take advantage of the interaction between electromagnetic
radiation and matter. In this chapter we turn our attention to electrochemical techniques in which the potential, current, or
charge in an electrochemical cell serves as the analytical signal. Although there are only three basic electrochemical signals,
there are a many possible experimental designs—too many, in fact, to cover adequately in an introductory textbook.
12.1: Overview of Electrochemistry
12.2: Potentiometric Methods
12.3: Coulometric Methods
12.4: Voltammetric Methods
12.5: Electrochemical Methods (Exercises)
12.6: Electrochemical Methods (Summary)
13: Chromatographic
For this reason, many analytical procedures include a step to separate the analyte from potential interferents. Although effective,
each additional step in an analytical procedure increases the analysis time and introduces uncertainty. In this chapter we
consider two analytical techniques that avoid these limitations by combining the separation and analysis: chromatography and
electrophoresis.
13.1: Overview of Analytical Separations
13.2: General Theory of Column Chromatography
13.3: Optimizing Chromatographic Separations
13.4: Gas Chromatography
13.5: High-Performance Liquid Chromatography
13.6: Other Forms of Liquid Chromatography
13.7: Electrophoresis
13.8: Chromatographic and Electrophoretic Methods (Exercises)
13.9: Chromatographic and Electrophoretic Methods (Summary)
14: Kinetic Methods
One way to classify analytical techniques is by whether the analyte’s concentration is determined by an equilibrium reaction or
by the kinetics of a chemical reaction or a physical process. Often analytical methods involve measurements made on systems
in which the analyte is always at equilibrium. In this chapter we turn our attention to measurements made under nonequilibrium conditions.
14.1: Kinetic Methods Versus Equilibrium Methods
14.2: Chemical Kinetics
14.3: Radiochemistry
14.4: Flow Injection Analysis
14.5: Kinetic Methods (Exercises)
14.6: Kinetic Methods (Summary)
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15: Developing a Standard Method
Among the goals of analytical chemistry are improving established methods of analysis, extending existing methods of analysis
to new types of samples, and developing new analytical methods. In this chapter we discuss how we develop a standard
method, including optimizing the experimental procedure, verifying that the method produces acceptable precision and
accuracy in the hands of a single analyst, and validating the method for general use.
15.1: Optimizing the Experimental Procedure
15.2: Verifying the Method
15.3: Validating the Method as a Standard Method
15.4: Using Excel and R for an Analysis of Variance
15.5: Developing a Standard Method (Exercises)
15.6: Developing a Standard Method (Summary)
16: Quality Assurance
Knowing that a method meets suitable standards is important if we are to have confidence in our results. Even so, using a
standard method does not guarantee that the result of an analysis is acceptable. In this chapter we introduce the quality
assurance procedures used in industry and government labs for monitoring routine chemical analyses.
16.1: The Analytical Perspective—Revisited
16.2: Quality Control
16.3: Quality Assessment
16.4: Evaluating Quality Assurance Data
16.5: Quality Assurance (Exercises)
17: Additional Resources
18: Back Matter
Table of Contents
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Index
A
alpha particle
abbreviation
3.1: Measurements in Analytical Chemistry
absorbance
4.3: Classifying Analytical Techniques
11.1: Overview of Spectroscopy
11.2: Spectroscopy Based on Absorption
15.1: Optimizing the Experimental Procedure
Absorbance Spectra
11.2: Spectroscopy Based on Absorption
absorbance spectrum
11.1: Overview of Spectroscopy
Absorption
11.2: Spectroscopy Based on Absorption
11.6: Photoluminescence Spectroscopy
absorption spectrophotometers
11.4: Atomic Absorption Spectroscopy
absorption spectroscopy
11.2: Spectroscopy Based on Absorption
11.4: Atomic Absorption Spectroscopy
absorption spectrum
13.5: High-Performance Liquid Chromatography
absorptivity
11.2: Spectroscopy Based on Absorption
15.1: Optimizing the Experimental Procedure
accuracy
4.4: Selecting an Analytical Method
5.2: Characterizing Experimental Errors
11.3: UV/Vis and IR Spectroscopy
11.4: Atomic Absorption Spectroscopy
11.7: Atomic Emission Spectroscopy
15.2: Verifying the Method
15.3: Validating the Method as a Standard Method
acetic acid
7.6: Ladder Diagrams
acid
7.4: Equilibrium Constants for Chemical Reactions
7.7: Solving Equilibrium Problems
7.8: Buffer Solutions
acid–base buffer
7.8: Buffer Solutions
acid–base titrations
10.2: Acid–Base Titrations
acid–base titrimetry
10.2: Acid–Base Titrations
10.4: Redox Titrations
acidity
10.2: Acid–Base Titrations
activity
7.9: Activity Effects
12.2: Potentiometric Methods
Activity Coefficients
7.9: Activity Effects
Activity Effects
7.9: Activity Effects
adjusted retention time
13.2: General Theory of Column Chromatography
adsorption chromatography
13.1: Overview of Analytical Separations
algorithm
15.1: Optimizing the Experimental Procedure
Alkalinity
10.2: Acid–Base Titrations
Analytical Columns
14.3: Radiochemistry
13.5: High-Performance Liquid Chromatography
alternative hypotheses
5.5: Statistical Analysis of Data
alternative hypothesis
5.5: Statistical Analysis of Data
amalgam
12.4: Voltammetric Methods
amperometry
12.1: Overview of Electrochemistry
12.4: Voltammetric Methods
13.5: High-Performance Liquid Chromatography
amphiprotic
7.4: Equilibrium Constants for Chemical Reactions
Amphiprotic Species
7.4: Equilibrium Constants for Chemical Reactions
amplitude
11.1: Overview of Spectroscopy
analysis
4.1: Analysis, Determination, and Measurement
14.1: Kinetic Methods Versus Equilibrium Methods
Analysis of Standards
16.3: Quality Assessment
Analysis of Variance
15.3: Validating the Method as a Standard Method
15.4: Using Excel and R for an Analysis of Variance
analyst
15.2: Verifying the Method
analysts
15.3: Validating the Method as a Standard Method
analyte
analytical data
16.1: The Analytical Perspective—Revisited
analytical method
2.1: What is Analytical Chemistry?
4.4: Selecting an Analytical Method
5.5: Statistical Analysis of Data
6.1: Analytical Standards
6.3: Determining the Sensitivity
7.6: Ladder Diagrams
8.4: Separating the Analyte from Interferents
11.3: UV/Vis and IR Spectroscopy
15.3: Validating the Method as a Standard Method
16.4: Evaluating Quality Assurance Data
analytical methodology
4.7: The Importance of Analytical Methodology
analytical methods
4.4: Selecting an Analytical Method
4.7: The Importance of Analytical Methodology
6.5: Blank Corrections
Analytical Perspective
16.1: The Analytical Perspective—Revisited
analytical separation
8.5: General Theory of Separation Efficiency
Analytical Separations
13.1: Overview of Analytical Separations
analytical signal
9.1: Overview of Gravimetric Methods
13.5: High-Performance Liquid Chromatography
14.1: Kinetic Methods Versus Equilibrium Methods
Analytical titrations
10.4: Redox Titrations
4.1: Analysis, Determination, and Measurement
8.5: General Theory of Separation Efficiency
9.2: Precipitation Gravimetry
9.4: Particulate Gravimetry
10.1: Overview of Titrimetry
11.3: UV/Vis and IR Spectroscopy
11.4: Atomic Absorption Spectroscopy
11.5: Emission Spectroscopy
12.1: Overview of Electrochemistry
12.2: Potentiometric Methods
12.3: Coulometric Methods
13.1: Overview of Analytical Separations
13.4: Gas Chromatography
15.1: Optimizing the Experimental Procedure
16.3: Quality Assessment
Analyte’s Concentration
13.4: Gas Chromatography
analytes
Analyze Data
5.8: Using Excel and R to Analyze Data
anodic current
12.4: Voltammetric Methods
anova
15.3: Validating the Method as a Standard Method
Applied Potential
12.4: Voltammetric Methods
aqueous buffer
13.7: Electrophoresis
argentometric titration
10.5: Precipitation Titrations
asymmetric equivalence point
10.4: Redox Titrations
Asymmetric Peaks
11.6: Photoluminescence Spectroscopy
13.7: Electrophoresis
analytical
14.1: Kinetic Methods Versus Equilibrium Methods
Analytical Approach
2.2: The Analytical Perspective
analytical balance
13.2: General Theory of Column Chromatography
Atomic emission
11.7: Atomic Emission Spectroscopy
Atomic Emission Spectra
11.7: Atomic Emission Spectroscopy
Atomic Emission Spectroscopy
11.7: Atomic Emission Spectroscopy
3.4: Basic Equipment
analytical calculations
3.3: Stoichiometric Calculations
analytical chemistry
2.1: What is Analytical Chemistry?
3.1: Measurements in Analytical Chemistry
12.1: Overview of Electrochemistry
analytical chemists
2.2: The Analytical Perspective
1
atomic number
14.3: Radiochemistry
Atomization
11.4: Atomic Absorption Spectroscopy
11.7: Atomic Emission Spectroscopy
Atomization Methods
11.4: Atomic Absorption Spectroscopy
attenuated total reflectance
11.3: UV/Vis and IR Spectroscopy
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auxiliary complexing agent
10.3: Complexation Titrations
auxiliary electrode
12.1: Overview of Electrochemistry
13.5: High-Performance Liquid Chromatography
auxiliary oxidizing agents
10.4: Redox Titrations
auxiliary reducing agent
10.4: Redox Titrations
average
5.6: Statistical Methods for Normal Distributions
calomel electrodes
chemical analysis
12.2: Potentiometric Methods
capillary
13.5: High-Performance Liquid Chromatography
13.7: Electrophoresis
Capillary Columns
capillary electrochromatography
13.7: Electrophoresis
Capillary Electrophoresis
capillary gel electrophoresis
background correction
11.4: Atomic Absorption Spectroscopy
balanced reaction
3.3: Stoichiometric Calculations
band broadening
13.2: General Theory of Column Chromatography
base
7.4: Equilibrium Constants for Chemical Reactions
baseline width
13.2: General Theory of Column Chromatography
Beer’s Law
11.2: Spectroscopy Based on Absorption
Berthollet
7.1: Reversible Reactions and Chemical Equilibria
beta particle
14.3: Radiochemistry
binomial distribution
5.4: The Distribution of Measurements and Results
blank
6.5: Blank Corrections
blind analysis
15.2: Verifying the Method
Bonded stationary phases
13.5: High-Performance Liquid Chromatography
box plot
5.8: Using Excel and R to Analyze Data
buffer
7.8: Buffer Solutions
13.7: Electrophoresis
buffer capacity
7.8: Buffer Solutions
Buffer Solutions
7.8: Buffer Solutions
buffer viscosity
13.7: Electrophoresis
Buret
10.1: Overview of Titrimetry
C
calculations
3.3: Stoichiometric Calculations
Calibration
4.5: Developing the Procedure
calibration curve
14.2: Chemical Kinetics
15.1: Optimizing the Experimental Procedure
Calibration Curves
6.4: Linear Regression and Calibration Curves
Calomel
12.2: Potentiometric Methods
11.4: Atomic Absorption Spectroscopy
11.7: Atomic Emission Spectroscopy
Chemical kinetic
13.3: Optimizing Chromatographic Separations
13.4: Gas Chromatography
13.7: Electrophoresis
B
2.1: What is Analytical Chemistry?
Chemical Interferences
13.7: Electrophoresis
14.2: Chemical Kinetics
14.4: Flow Injection Analysis
Chemical kinetic methods
14.2: Chemical Kinetics
14.4: Flow Injection Analysis
chemical kinetics
14.2: Chemical Kinetics
Chemical Properties
8.6: Classifying Separation Techniques
capillary tubing
chemical reaction
13.7: Electrophoresis
Capillary Zone Electrophoresis
13.7: Electrophoresis
7.2: Thermodynamics and Equilibrium Chemistry
14.2: Chemical Kinetics
chemiluminescence
capillary’s radius
11.1: Overview of Spectroscopy
13.7: Electrophoresis
Chesapeake Bay Monitoring Program
Catalytic activity
4.7: The Importance of Analytical Methodology
14.2: Chemical Kinetics
chromatogram
cathode
12.2: Potentiometric Methods
cathodic current
12.4: Voltammetric Methods
CCB
13.4: Gas Chromatography
Chromatographic
13.2: General Theory of Column Chromatography
Chromatographic Columns
13.4: Gas Chromatography
4.6: Protocols
Chromatographic Resolution
CCV
13.2: General Theory of Column Chromatography
4.6: Protocols
chromatography
CEC
13.7: Electrophoresis
central composite design
15.1: Optimizing the Experimental Procedure
Central Limit Theorem
5.4: The Distribution of Measurements and Results
Central Tendency
5.1: Characterizing Measurements and Results
centrifugal analyzer
8.6: Classifying Separation Techniques
13.1: Overview of Analytical Separations
13.2: General Theory of Column Chromatography
13.4: Gas Chromatography
13.5: High-Performance Liquid Chromatography
13.6: Other Forms of Liquid Chromatography
Claude Berthollet
7.1: Reversible Reactions and Chemical Equilibria
Clinical
11.3: UV/Vis and IR Spectroscopy
14.2: Chemical Kinetics
coagulation
centrifugation
8.6: Classifying Separation Techniques
CGE
9.2: Precipitation Gravimetry
Collaborative Study
15.3: Validating the Method as a Standard Method
13.7: Electrophoresis
collaborative test
characteristic decay
15.3: Validating the Method as a Standard Method
14.3: Radiochemistry
Collaborative Testing
Characterization
10.2: Acid–Base Titrations
11.3: UV/Vis and IR Spectroscopy
12.3: Coulometric Methods
12.4: Voltammetric Methods
14.2: Chemical Kinetics
14.3: Radiochemistry
characterization analysis
2.3: Common Analytical Problems
charge
12.3: Coulometric Methods
charge balance
15.3: Validating the Method as a Standard Method
column
13.6: Other Forms of Liquid Chromatography
column chromatography
13.1: Overview of Analytical Separations
13.2: General Theory of Column Chromatography
column efficiency
13.2: General Theory of Column Chromatography
13.3: Optimizing Chromatographic Separations
Columns
13.5: High-Performance Liquid Chromatography
7.7: Solving Equilibrium Problems
charge balance equation
7.7: Solving Equilibrium Problems
charging current
common ion effect
7.7: Solving Equilibrium Problems
competitive inhibition
14.2: Chemical Kinetics
12.4: Voltammetric Methods
Chauvenet’s criterion
5.6: Statistical Methods for Normal Distributions
2
Complexation
7.4: Equilibrium Constants for Chemical Reactions
7.6: Ladder Diagrams
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Complexation Reactions
convection
7.4: Equilibrium Constants for Chemical Reactions
complexation titrations
10.3: Complexation Titrations
Complexation Titrimetry
10.3: Complexation Titrations
composite sample
8.2: Designing a Sampling Plan
concentration
3.2: Concentration
3.4: Basic Equipment
5.7: Detection Limits
6.4: Linear Regression and Calibration Curves
7.7: Solving Equilibrium Problems
7.9: Activity Effects
7.10: Using Excel and R to Solve Equilibrium
Problems
8.5: General Theory of Separation Efficiency
9.2: Precipitation Gravimetry
10.2: Acid–Base Titrations
11.8: Spectroscopy Based on Scattering
12.2: Potentiometric Methods
12.3: Coulometric Methods
12.4: Voltammetric Methods
13.1: Overview of Analytical Separations
13.4: Gas Chromatography
13.7: Electrophoresis
14.2: Chemical Kinetics
14.4: Flow Injection Analysis
15.1: Optimizing the Experimental Procedure
15.2: Verifying the Method
16.3: Quality Assessment
convenience sampling
8.2: Designing a Sampling Plan
coprecipitates
9.2: Precipitation Gravimetry
corresponding
7.8: Buffer Solutions
14.4: Flow Injection Analysis
4.3: Classifying Analytical Techniques
concentrations
10.2: Acid–Base Titrations
10.4: Redox Titrations
12.1: Overview of Electrochemistry
16.4: Evaluating Quality Assurance Data
4.4: Selecting an Analytical Method
coulombs
12.3: Coulometric Methods
coulometric titration
12.3: Coulometric Methods
Coulometric Titrations
12.3: Coulometric Methods
coulometry
12.3: Coulometric Methods
13.5: High-Performance Liquid Chromatography
counter electrode
12.1: Overview of Electrochemistry
countercurrent extraction
13.1: Overview of Analytical Separations
cryogenic focusing
13.4: Gas Chromatography
Current
12.1: Overview of Electrochemistry
12.4: Voltammetric Methods
Current efficiency
10.3: Complexation Titrations
conductivity
13.5: High-Performance Liquid Chromatography
Confidence Interval
5.5: Statistical Analysis of Data
15.3: Validating the Method as a Standard Method
Confidence Intervals
5.4: The Distribution of Measurements and Results
coning
8.3: Implementing the Sampling Plan
conservation of mass
9.1: Overview of Gravimetric Methods
constant determinate error
5.2: Characterizing Experimental Errors
Constant Potential
12.3: Coulometric Methods
continuing calibration blank
4.6: Protocols
continuing calibration verification
4.6: Protocols
contour map
15.1: Optimizing the Experimental Procedure
Contract Laboratory Program
4.6: Protocols
control chart
16.4: Evaluating Quality Assurance Data
15.2: Verifying the Method
detection limit
4.4: Selecting an Analytical Method
5.7: Detection Limits
15.2: Verifying the Method
16.4: Evaluating Quality Assurance Data
14.4: Flow Injection Analysis
Detectors
13.5: High-Performance Liquid Chromatography
13.7: Electrophoresis
determinate error
5.2: Characterizing Experimental Errors
Determination
4.1: Analysis, Determination, and Measurement
5.4: The Distribution of Measurements and Results
Dialysis
8.6: Classifying Separation Techniques
14.4: Flow Injection Analysis
diffusion
12.4: Voltammetric Methods
14.4: Flow Injection Analysis
diffusion layer
12.4: Voltammetric Methods
Digestion
9.2: Precipitation Gravimetry
dilution
3.5: Preparing Solutions
12.3: Coulometric Methods
curve fitting
Diode Array Spectrometer
11.3: UV/Vis and IR Spectroscopy
14.2: Chemical Kinetics
Curvilinear regression
6.4: Linear Regression and Calibration Curves
Cyclic Voltammetry
direct analysis
9.1: Overview of Gravimetric Methods
direct titration
10.1: Overview of Titrimetry
12.4: Voltammetric Methods
conditional formation constant
3.4: Basic Equipment
detection
Detector
Cost
concentration gradient
concentration techniques
desiccator
12.4: Voltammetric Methods
14.4: Flow Injection Analysis
dispersion
14.4: Flow Injection Analysis
D
displacement titration
dark current
10.1: Overview of Titrimetry
11.1: Overview of Spectroscopy
Data
5.5: Statistical Analysis of Data
5.8: Using Excel and R to Analyze Data
Data Analysis
5.8: Using Excel and R to Analyze Data
6.6: Using Excel and R for a Regression Analysis
15.4: Using Excel and R for an Analysis of Variance
definitive techniques
9.1: Overview of Gravimetric Methods
degrees of freedom
5.4: The Distribution of Measurements and Results
15.3: Validating the Method as a Standard Method
density
8.6: Classifying Separation Techniques
density gradient centrifugation
8.6: Classifying Separation Techniques
dependent
15.1: Optimizing the Experimental Procedure
dependent factors
15.1: Optimizing the Experimental Procedure
Descriptive Statistics
5.8: Using Excel and R to Analyze Data
desiccant
dissociation
7.4: Equilibrium Constants for Chemical Reactions
7.8: Buffer Solutions
dissociation constant
7.4: Equilibrium Constants for Chemical Reactions
7.8: Buffer Solutions
distillation
8.6: Classifying Separation Techniques
Distribution of Measurements
5.4: The Distribution of Measurements and Results
Distribution Ratios
8.7: Liquid–Liquid Extractions
Dixon’s Q‑test
5.6: Statistical Methods for Normal Distributions
DME
12.4: Voltammetric Methods
dot chart
5.8: Using Excel and R to Analyze Data
dropping mercury electrode
12.4: Voltammetric Methods
Drying
3.4: Basic Equipment
duplicate samples
16.3: Quality Assessment
3.4: Basic Equipment
3
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E
electroosmotic flow velocity
ECD
13.4: Gas Chromatography
EDTA
10.3: Complexation Titrations
effective
15.1: Optimizing the Experimental Procedure
effective bandwidth
11.1: Overview of Spectroscopy
effective electric
13.7: Electrophoresis
effective electric field
13.7: Electrophoresis
effectiveness
15.1: Optimizing the Experimental Procedure
Efficiency
13.7: Electrophoresis
15.1: Optimizing the Experimental Procedure
electrochemical cell
12.3: Coulometric Methods
12.4: Voltammetric Methods
electrochemical cells
12.2: Potentiometric Methods
Electrochemical Detectors
13.5: High-Performance Liquid Chromatography
electrochemical measurements
13.5: High-Performance Liquid Chromatography
Electrochemical Techniques
12.1: Overview of Electrochemistry
electrochemically irreversible
12.4: Voltammetric Methods
electrochemically reversible
12.4: Voltammetric Methods
electrochemistry
4.3: Classifying Analytical Techniques
12.1: Overview of Electrochemistry
electrode
12.1: Overview of Electrochemistry
12.2: Potentiometric Methods
12.3: Coulometric Methods
electrode’s potential
12.3: Coulometric Methods
electrodes
12.2: Potentiometric Methods
Electrogravimetry
9.1: Overview of Gravimetric Methods
12.3: Coulometric Methods
electrokinetic injection
13.7: Electrophoresis
electrolysis
12.3: Coulometric Methods
Electrolysis Time
12.3: Coulometric Methods
electromagnetic radiation
11.1: Overview of Spectroscopy
11.2: Spectroscopy Based on Absorption
15.1: Optimizing the Experimental Procedure
electromagnetic spectrum
11.1: Overview of Spectroscopy
electron capture detector
13.4: Gas Chromatography
electroosmotic
13.7: Electrophoresis
electroosmotic flow
13.7: Electrophoresis
equilibrium constan
7.3: Manipulating Equilibrium Constants
electropherogram
equilibrium constant
13.7: Electrophoresis
7.2: Thermodynamics and Equilibrium Chemistry
7.3: Manipulating Equilibrium Constants
12.2: Potentiometric Methods
electrophoresis
13.7: Electrophoresis
Equilibrium Constants
Electrophoretic
13.1: Overview of Analytical Separations
Electrophoretic Mobility
13.7: Electrophoresis
Electrophoretic Separations
13.1: Overview of Analytical Separations
electrophoretic velocity
13.7: Electrophoresis
7.3: Manipulating Equilibrium Constants
10.2: Acid–Base Titrations
11.3: UV/Vis and IR Spectroscopy
equilibrium method
14.1: Kinetic Methods Versus Equilibrium Methods
equilibrium reaction
8.7: Liquid–Liquid Extractions
14.1: Kinetic Methods Versus Equilibrium Methods
Equipment
emission
11.1: Overview of Spectroscopy
14.3: Radiochemistry
emission spectra
11.6: Photoluminescence Spectroscopy
11.7: Atomic Emission Spectroscopy
Emission Spectroscopy
11.7: Atomic Emission Spectroscopy
emission spectrum
11.6: Photoluminescence Spectroscopy
empirical model
15.1: Optimizing the Experimental Procedure
End point
10.2: Acid–Base Titrations
10.3: Complexation Titrations
10.5: Precipitation Titrations
End points
10.1: Overview of Titrimetry
Endpoint
12.3: Coulometric Methods
enthalpy
7.2: Thermodynamics and Equilibrium Chemistry
entropy
7.2: Thermodynamics and Equilibrium Chemistry
environmental monitoring programs
4.7: The Importance of Analytical Methodology
Enzyme Catalysis
14.2: Chemical Kinetics
enzyme electrodes
12.2: Potentiometric Methods
Enzymes
4.4: Selecting an Analytical Method
equivalence
10.1: Overview of Titrimetry
10.2: Acid–Base Titrations
equivalence point
10.1: Overview of Titrimetry
10.2: Acid–Base Titrations
10.4: Redox Titrations
Equivalence Points
10.1: Overview of Titrimetry
Equivalency Testing
15.2: Verifying the Method
Equivalent Weights
10.2: Acid–Base Titrations
error
5.2: Characterizing Experimental Errors
15.3: Validating the Method as a Standard Method
errors
16.4: Evaluating Quality Assurance Data
Ethylenediaminetetraacetic
10.3: Complexation Titrations
ethylenediaminetetraacetic acid
10.3: Complexation Titrations
Excel
3.6: Spreadsheets and Computational Software
5.8: Using Excel and R to Analyze Data
6.6: Using Excel and R for a Regression Analysis
15.4: Using Excel and R for an Analysis of Variance
Excitation
11.2: Spectroscopy Based on Absorption
11.7: Atomic Emission Spectroscopy
excitation spectrum
14.2: Chemical Kinetics
Equilibria
11.6: Photoluminescence Spectroscopy
exclusion limit
7.6: Ladder Diagrams
equilibrium
13.6: Other Forms of Liquid Chromatography
7.1: Reversible Reactions and Chemical Equilibria
7.3: Manipulating Equilibrium Constants
7.5: Le Châtelier’s Principle
7.6: Ladder Diagrams
7.7: Solving Equilibrium Problems
7.9: Activity Effects
7.10: Using Excel and R to Solve Equilibrium
Problems
8.7: Liquid–Liquid Extractions
11.3: UV/Vis and IR Spectroscopy
12.1: Overview of Electrochemistry
equilibrium chemistry
7.6: Ladder Diagrams
equilibrium concentration
Experimental Errors
5.2: Characterizing Experimental Errors
external conversion
11.6: Photoluminescence Spectroscopy
External Standards
6.3: Determining the Sensitivity
12.2: Potentiometric Methods
extraction
8.6: Classifying Separation Techniques
8.7: Liquid–Liquid Extractions
Extraction efficiency
8.7: Liquid–Liquid Extractions
7.7: Solving Equilibrium Problems
7.10: Using Excel and R to Solve Equilibrium
Problems
13.7: Electrophoresis
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F
Fourier transform spectrometer
factor levels
15.1: Optimizing the Experimental Procedure
Factorial
15.1: Optimizing the Experimental Procedure
Factorial Designs
15.1: Optimizing the Experimental Procedure
factors
15.1: Optimizing the Experimental Procedure
15.2: Verifying the Method
Fajans method
10.5: Precipitation Titrations
faradaic current
12.4: Voltammetric Methods
Faraday’s constant
12.3: Coulometric Methods
Faraday’s law
12.3: Coulometric Methods
fiagram
14.4: Flow Injection Analysis
FID
13.4: Gas Chromatography
field blank
16.3: Quality Assessment
16.4: Evaluating Quality Assurance Data
filter
11.1: Overview of Spectroscopy
Filter Photometer
11.3: UV/Vis and IR Spectroscopy
filtrate
8.6: Classifying Separation Techniques
filtration
8.6: Classifying Separation Techniques
Flame Atomizer
11.4: Atomic Absorption Spectroscopy
Flame Ionization Detector
13.4: Gas Chromatography
flow injection
14.4: Flow Injection Analysis
flow injection analysis
14.4: Flow Injection Analysis
flow injection analyzer
14.4: Flow Injection Analysis
fluorescence
11.6: Photoluminescence Spectroscopy
Fluorescence spectra
11.6: Photoluminescence Spectroscopy
fluorescent
11.6: Photoluminescence Spectroscopy
13.5: High-Performance Liquid Chromatography
fluorescent quantum yield
11.6: Photoluminescence Spectroscopy
fluorimeter
11.6: Photoluminescence Spectroscopy
Forensic
11.3: UV/Vis and IR Spectroscopy
formality
3.2: Concentration
formation constant
7.4: Equilibrium Constants for Chemical Reactions
14.1: Kinetic Methods Versus Equilibrium Methods
Gravimetry
11.3: UV/Vis and IR Spectroscopy
4.3: Classifying Analytical Techniques
9: Gravimetric Methods
9.1: Overview of Gravimetric Methods
9.2: Precipitation Gravimetry
9.3: Volatilization Gravimetry
9.4: Particulate Gravimetry
frequency
11.1: Overview of Spectroscopy
fundamental analysis
2.3: Common Analytical Problems
G
gross sample
8.3: Implementing the Sampling Plan
Grubb’s test
galvanostat
12.1: Overview of Electrochemistry
Galvanostats
12.1: Overview of Electrochemistry
gamma ray
5.6: Statistical Methods for Normal Distributions
GSC
13.4: Gas Chromatography
Guard columns
13.5: High-Performance Liquid Chromatography
14.3: Radiochemistry
gas
8.3: Implementing the Sampling Plan
13.4: Gas Chromatography
gas chromatography
H
hanging mercury drop electrode
12.4: Voltammetric Methods
13.3: Optimizing Chromatographic Separations
13.4: Gas Chromatography
Gas–Liquid Chromatography
13.4: Gas Chromatography
gaseous diffusion
14.4: Flow Injection Analysis
Gases
8.3: Implementing the Sampling Plan
Gaussian
13.2: General Theory of Column Chromatography
GC detectors
13.6: Other Forms of Liquid Chromatography
Geiger counter
headspace sampling
13.4: Gas Chromatography
Henderson–Hasselbalch approximation
7.8: Buffer Solutions
heterogeneous
8.2: Designing a Sampling Plan
histogram
5.4: The Distribution of Measurements and Results
HMDE
12.4: Voltammetric Methods
homogeneous
8.2: Designing a Sampling Plan
homogeneous precipitation
14.3: Radiochemistry
general elution problem
13.3: Optimizing Chromatographic Separations
Gibb’s free energy
7.2: Thermodynamics and Equilibrium Chemistry
glass electrodes
12.2: Potentiometric Methods
GLC
13.4: Gas Chromatography
global optimum
15.1: Optimizing the Experimental Procedure
GMP
9.2: Precipitation Gravimetry
HPLC
13.5: High-Performance Liquid Chromatography
HPLC column
13.6: Other Forms of Liquid Chromatography
HPLC detectors
13.5: High-Performance Liquid Chromatography
HPLC Plumbing
13.5: High-Performance Liquid Chromatography
Hydrodynamic injection
13.7: Electrophoresis
hydrodynamic voltammetry
16.2: Quality Control
12.4: Voltammetric Methods
GMPs
16.2: Quality Control
Good laboratory practices
16.2: Quality Control
Good measurement practices
16.2: Quality Control
I
ICB
4.6: Protocols
ICV
4.6: Protocols
grab sample
8.2: Designing a Sampling Plan
gradient elutions
13.5: High-Performance Liquid Chromatography
graphite furnace
11.4: Atomic Absorption Spectroscopy
gravimetric analysis
ICV and
4.6: Protocols
ignition
9.2: Precipitation Gravimetry
Ilkovic equation
12.4: Voltammetric Methods
In situ sampling
9: Gravimetric Methods
8.2: Designing a Sampling Plan
gravimetric method
4.4: Selecting an Analytical Method
Incident Radiation
11.8: Spectroscopy Based on Scattering
inclusion
Formation constants
9.2: Precipitation Gravimetry
10.3: Complexation Titrations
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inclusion limit
IR Spectroscopy
13.6: Other Forms of Liquid Chromatography
Independent
isocratic elution
15.1: Optimizing the Experimental Procedure
independent factors
13.5: High-Performance Liquid Chromatography
10.1: Overview of Titrimetry
10.2: Acid–Base Titrations
10.5: Precipitation Titrations
12.2: Potentiometric Methods
indicator electrode
12.1: Overview of Electrochemistry
Indicator Electrodes
12.2: Potentiometric Methods
indirect analysis
9.1: Overview of Gravimetric Methods
Infrared Spectra
11.2: Spectroscopy Based on Absorption
inhibitor
13.4: Gas Chromatography
initial calibration blank
4.6: Protocols
initial calibration verification
14.3: Radiochemistry
14.3: Radiochemistry
14.2: Chemical Kinetics
9.3: Volatilization Gravimetry
Instrumentation
11.3: UV/Vis and IR Spectroscopy
11.6: Photoluminescence Spectroscopy
12.3: Coulometric Methods
14.3: Radiochemistry
14.4: Flow Injection Analysis
integrated rate law
14.2: Chemical Kinetics
12.1: Overview of Electrochemistry
12.1: Overview of Electrochemistry
Interferences
4.5: Developing the Procedure
interferent
4.4: Selecting an Analytical Method
interferogram
11.1: Overview of Spectroscopy
interferometer
11.1: Overview of Spectroscopy
Interferometers
11.1: Overview of Spectroscopy
internal conversion
11.6: Photoluminescence Spectroscopy
internal standard
6.3: Determining the Sensitivity
intersystem crossing
11.6: Photoluminescence Spectroscopy
ionic strength
7.9: Activity Effects
ionization suppressor
11.4: Atomic Absorption Spectroscopy
IR spectra
11.2: Spectroscopy Based on Absorption
13.1: Overview of Analytical Separations
liquid–solid adsorption chromatography
J
13.6: Other Forms of Liquid Chromatography
local optimum
Jones reductor
15.1: Optimizing the Experimental Procedure
10.4: Redox Titrations
longitudinal diffusion
Joule heating
13.3: Optimizing Chromatographic Separations
13.7: Electrophoresis
judgmental sampling
8.2: Designing a Sampling Plan
junction potential
12.2: Potentiometric Methods
loop injector
13.5: High-Performance Liquid Chromatography
LSC
13.6: Other Forms of Liquid Chromatography
M
K
manifold
Ka
4.4: Selecting an Analytical Method
6.4: Linear Regression and Calibration Curves
7.4: Equilibrium Constants for Chemical Reactions
Kb
7.4: Equilibrium Constants for Chemical Reactions
KD
8.6: Classifying Separation Techniques
kernel density plot
5.8: Using Excel and R to Analyze Data
kinetic method
14.1: Kinetic Methods Versus Equilibrium Methods
Kjeldahl analysis
10.2: Acid–Base Titrations
Interfacial
Interfacial Concentrations
13.5: High-Performance Liquid Chromatography
Liquid–Liquid Extractions
5.7: Detection Limits
initial rate
Inorganic Analysis
13.5: High-Performance Liquid Chromatography
liquid mobile phase
IUPAC
4.6: Protocols
6.4: Linear Regression and Calibration Curves
liquid chromatography
isotopes
14.2: Chemical Kinetics
12.4: Voltammetric Methods
Linear Regression
isotope dilution
5.2: Characterizing Experimental Errors
indicator
5.7: Detection Limits
limiting current
isothermal
15.1: Optimizing the Experimental Procedure
indeterminate errors
limit of identification
11.3: UV/Vis and IR Spectroscopy
14.4: Flow Injection Analysis
mass
3.4: Basic Equipment
4.3: Classifying Analytical Techniques
5.1: Characterizing Measurements and Results
8.6: Classifying Separation Techniques
9.1: Overview of Gravimetric Methods
mass spectrometer
13.4: Gas Chromatography
mass spectrum
13.4: Gas Chromatography
Mass Transfer
13.3: Optimizing Chromatographic Separations
mass transport
12.4: Voltammetric Methods
L
Mathematical
laboratory
3.7: The Laboratory Notebook
laboratory notebook
3.7: The Laboratory Notebook
laboratory sample
8.3: Implementing the Sampling Plan
Ladder diagram
7.6: Ladder Diagrams
12.3: Coulometric Methods
Ladder diagrams
7.8: Buffer Solutions
laminar flow
15.1: Optimizing the Experimental Procedure
Mathematical Models
15.1: Optimizing the Experimental Procedure
matrix
4.1: Analysis, Determination, and Measurement
matrix matching
6.3: Determining the Sensitivity
mean
5.1: Characterizing Measurements and Results
5.6: Statistical Methods for Normal Distributions
15.3: Validating the Method as a Standard Method
measurement
14.4: Flow Injection Analysis
Le Châtelier’s principle
7.5: Le Châtelier’s Principle
7.6: Ladder Diagrams
Le Chatelier's Principle
7.5: Le Châtelier’s Principle
leveling
10.2: Acid–Base Titrations
lifetime
11.5: Emission Spectroscopy
ligand
4.1: Analysis, Determination, and Measurement
5.1: Characterizing Measurements and Results
5.2: Characterizing Experimental Errors
Measurement Errors
5.2: Characterizing Experimental Errors
measurements
3.1: Measurements in Analytical Chemistry
5.4: The Distribution of Measurements and Results
12.2: Potentiometric Methods
15.1: Optimizing the Experimental Procedure
Measuring Volume
3.4: Basic Equipment
7.4: Equilibrium Constants for Chemical Reactions
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median
molarity
5.1: Characterizing Measurements and Results
medication
normality
3.2: Concentration
3.2: Concentration
Moles
5.5: Statistical Analysis of Data
notebook
3.3: Stoichiometric Calculations
MEKC
Monitoring Absorbance
13.7: Electrophoresis
3.7: The Laboratory Notebook
Nuclear Reactor
10.3: Complexation Titrations
Membrane Electrodes
monitoring program
12.2: Potentiometric Methods
14.3: Radiochemistry
Nyquist theorem
4.7: The Importance of Analytical Methodology
membrane potential
monochromatic
12.2: Potentiometric Methods
11.1: Overview of Spectroscopy
11.8: Spectroscopy Based on Scattering
Membrane Potentials
monochromator
12.2: Potentiometric Methods
11.1: Overview of Spectroscopy
Membranes
Monolithic columns
12.2: Potentiometric Methods
13.5: High-Performance Liquid Chromatography
meniscus
Monoprotic
3.4: Basic Equipment
7.4: Equilibrium Constants for Chemical Reactions
7.7: Solving Equilibrium Problems
mercury film electrode
12.4: Voltammetric Methods
MS
metallochromic indicators
13.4: Gas Chromatography
10.3: Complexation Titrations
Multicomponent Analysis
method
4.2: Techniques, Methods, Procedures, and Protocols
4.4: Selecting an Analytical Method
6.3: Determining the Sensitivity
method blank
12.4: Voltammetric Methods
Multielemental Analysis
11.7: Atomic Emission Spectroscopy
multiple paths
4.5: Developing the Procedure
16.3: Quality Assessment
13.3: Optimizing Chromatographic Separations
Multivariate Regression
method error
6.4: Linear Regression and Calibration Curves
8.2: Designing a Sampling Plan
O
Occlusions
9.2: Precipitation Gravimetry
Ohm’s law
12.1: Overview of Electrochemistry
open tubular column
13.4: Gas Chromatography
Optimization
15.1: Optimizing the Experimental Procedure
Optimize Resolution
13.3: Optimizing Chromatographic Separations
Organic Analysis
9.3: Volatilization Gravimetry
Outliers
5.6: Statistical Methods for Normal Distributions
overpotential
12.3: Coulometric Methods
oxidation
7.4: Equilibrium Constants for Chemical Reactions
7.6: Ladder Diagrams
5.2: Characterizing Experimental Errors
Method Errors
N
5.2: Characterizing Experimental Errors
method of continuous variations
12.2: Potentiometric Methods
14.3: Radiochemistry
11.3: UV/Vis and IR Spectroscopy
oxidizing agent
Nephelometry
method of standard additions
7.4: Equilibrium Constants for Chemical Reactions
11.8: Spectroscopy Based on Scattering
6.3: Determining the Sensitivity
Micellar
electrokinetic
chromatography
oxidation reaction
negatron
capillary
13.7: Electrophoresis
Micelle
13.7: Electrophoresis
Michaelis constant
14.2: Chemical Kinetics
microextraction
13.4: Gas Chromatography
Microsoft Excel
3.6: Spreadsheets and Computational Software
migration
12.4: Voltammetric Methods
Migration Time
13.7: Electrophoresis
mobile phase
13.1: Overview of Analytical Separations
13.4: Gas Chromatography
13.5: High-Performance Liquid Chromatography
13.6: Other Forms of Liquid Chromatography
Mobile Phases
13.1: Overview of Analytical Separations
Mobility
13.7: Electrophoresis
Mohr method
10.5: Precipitation Titrations
molar absorptivity
11.2: Spectroscopy Based on Absorption
15.1: Optimizing the Experimental Procedure
Nernst Equation
7.4: Equilibrium Constants for Chemical Reactions
12.2: Potentiometric Methods
Nessler
11.1: Overview of Spectroscopy
neutron
P
Packed columns
13.4: Gas Chromatography
paired data
5.6: Statistical Methods for Normal Distributions
Participate
14.3: Radiochemistry
12.1: Overview of Electrochemistry
neutron activation
Particulate gravimetry
14.3: Radiochemistry
Neutron Activation Analysis
14.3: Radiochemistry
9.1: Overview of Gravimetric Methods
9.4: Particulate Gravimetry
particulates
neutron flux
9.4: Particulate Gravimetry
14.3: Radiochemistry
partition coefficient
nominal wavelength
11.1: Overview of Spectroscopy
Noncatalytic Reactions
14.2: Chemical Kinetics
Noncompetitive Inhibition
14.2: Chemical Kinetics
8.6: Classifying Separation Techniques
Partition Coefficients
8.7: Liquid–Liquid Extractions
parts per billion
3.2: Concentration
Parts per million
nonfaradaic current
12.4: Voltammetric Methods
nonretained solutes
13.2: General Theory of Column Chromatography
normal calibration curve
6.3: Determining the Sensitivity
normal distribution
5.4: The Distribution of Measurements and Results
5.5: Statistical Analysis of Data
5.6: Statistical Methods for Normal Distributions
Normal Distributions
5.6: Statistical Methods for Normal Distributions
7
3.2: Concentration
pathlength
15.1: Optimizing the Experimental Procedure
peak capacity
13.2: General Theory of Column Chromatography
peak current
12.4: Voltammetric Methods
Peak height
14.4: Flow Injection Analysis
peak shape
13.2: General Theory of Column Chromatography
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peptization
9.2: Precipitation Gravimetry
personal error
5.2: Characterizing Experimental Errors
pH
7.4: Equilibrium Constants for Chemical Reactions
7.10: Using Excel and R to Solve Equilibrium
Problems
10.2: Acid–Base Titrations
12.2: Potentiometric Methods
pH scale
7.4: Equilibrium Constants for Chemical Reactions
phase angle
11.1: Overview of Spectroscopy
phosphorescence
11.6: Photoluminescence Spectroscopy
Phosphorescence Spectra
11.6: Photoluminescence Spectroscopy
phosphorescent
11.6: Photoluminescence Spectroscopy
phosphorescent quantum yield
11.6: Photoluminescence Spectroscopy
photodiode array
11.1: Overview of Spectroscopy
Photoluminescence
11.1: Overview of Spectroscopy
11.5: Emission Spectroscopy
11.6: Photoluminescence Spectroscopy
Photoluminescence spectroscopy
11.6: Photoluminescence Spectroscopy
photon
11.1: Overview of Spectroscopy
11.2: Spectroscopy Based on Absorption
Photon Transducers
11.1: Overview of Spectroscopy
photons
11.1: Overview of Spectroscopy
physical properties
8.6: Classifying Separation Techniques
pipet
3.4: Basic Equipment
planar chromatography
13.1: Overview of Analytical Separations
plasma
11.7: Atomic Emission Spectroscopy
PLOT
6.6: Using Excel and R for a Regression Analysis
13.4: Gas Chromatography
Plumbing
13.5: High-Performance Liquid Chromatography
pnorm
5.8: Using Excel and R to Analyze Data
point
10.2: Acid–Base Titrations
polarity index
13.5: High-Performance Liquid Chromatography
polarography
12.4: Voltammetric Methods
polychromatic
11.1: Overview of Spectroscopy
Polyprotic
7.4: Equilibrium Constants for Chemical Reactions
7.7: Solving Equilibrium Problems
population
Preconcentration
5.4: The Distribution of Measurements and Results
8.1: The Importance of Sampling
8.2: Designing a Sampling Plan
Populations
5.4: The Distribution of Measurements and Results
Positron
8.8: Separation Versus Preconcentration
Prescriptive Approach
16.4: Evaluating Quality Assurance Data
pressure
7.2: Thermodynamics and Equilibrium Chemistry
primary standard
14.3: Radiochemistry
6.1: Analytical Standards
potential
12.1: Overview of Electrochemistry
12.2: Potentiometric Methods
12.4: Voltammetric Methods
potential interferents
13.1: Overview of Analytical Separations
potentiometer
12.1: Overview of Electrochemistry
Potentiometric
12.2: Potentiometric Methods
Potentiometric Biosensors
12.2: Potentiometric Methods
Potentiometric Measurements
12.2: Potentiometric Methods
potentiometric method
12.3: Coulometric Methods
Potentiometric Methods
12.2: Potentiometric Methods
potentiometric titration curve
10.2: Acid–Base Titrations
potentiometry
12.2: Potentiometric Methods
potentiostat
12.1: Overview of Electrochemistry
Potentiostats
12.1: Overview of Electrochemistry
ppb
Probability Distributions
5.4: The Distribution of Measurements and Results
5.8: Using Excel and R to Analyze Data
procedure
4.2: Techniques, Methods, Procedures, and Protocols
product
7.5: Le Châtelier’s Principle
products
3.3: Stoichiometric Calculations
7.5: Le Châtelier’s Principle
proficiency standards
16.3: Quality Assessment
propagation of uncertainty
5.3: Propagation of Uncertainty
Property Control Chart
16.4: Evaluating Quality Assurance Data
proportional determinate error
5.2: Characterizing Experimental Errors
protocol
4.2: Techniques, Methods, Procedures, and Protocols
protocol for a specific purpose
16.2: Quality Control
proton
14.3: Radiochemistry
PSP
16.2: Quality Control
pulse polarography
3.2: Concentration
12.4: Voltammetric Methods
ppm
3.2: Concentration
Q
precipitant
9.2: Precipitation Gravimetry
precipitate
7.4: Equilibrium Constants for Chemical Reactions
9.2: Precipitation Gravimetry
precipitation
9.2: Precipitation Gravimetry
9.4: Particulate Gravimetry
10.1: Overview of Titrimetry
10.5: Precipitation Titrations
precipitation gravimetry
9.1: Overview of Gravimetric Methods
9.2: Precipitation Gravimetry
Precipitation Reactions
7.4: Equilibrium Constants for Chemical Reactions
precipitation titration
10.5: Precipitation Titrations
Precipitation Titrimetry
10.5: Precipitation Titrations
precision
4.4: Selecting an Analytical Method
5.2: Characterizing Experimental Errors
9.2: Precipitation Gravimetry
10.2: Acid–Base Titrations
11.3: UV/Vis and IR Spectroscopy
11.4: Atomic Absorption Spectroscopy
11.7: Atomic Emission Spectroscopy
15.2: Verifying the Method
15.3: Validating the Method as a Standard Method
16.4: Evaluating Quality Assurance Data
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qualitative analysis
2.3: Common Analytical Problems
Qualitative Applications
9.2: Precipitation Gravimetry
11.3: UV/Vis and IR Spectroscopy
quality assessment
16.1: The Analytical Perspective—Revisited
16.3: Quality Assessment
16.4: Evaluating Quality Assurance Data
quality assurance
4.6: Protocols
quality assurance program
16.1: The Analytical Perspective—Revisited
16.4: Evaluating Quality Assurance Data
quality control
4.6: Protocols
16.1: The Analytical Perspective—Revisited
16.2: Quality Control
Quantitative Analysis
2.3: Common Analytical Problems
Quantitative Applications
11.7: Atomic Emission Spectroscopy
12.3: Coulometric Methods
quantitative estimates
16.4: Evaluating Quality Assurance Data
quantitative science
3.1: Measurements in Analytical Chemistry
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quantitative transfer
3.5: Preparing Solutions
quartering
8.3: Implementing the Sampling Plan
quartz crystal microbalance
9.4: Particulate Gravimetry
quench
14.2: Chemical Kinetics
S
Redox
10.4: Redox Titrations
12.2: Potentiometric Methods
Redox Electrodes
12.2: Potentiometric Methods
redox indicator
10.4: Redox Titrations
Redox titration
Redox Titration Curves
10.4: Redox Titrations
R
5.8: Using Excel and R to Analyze Data
15.4: Using Excel and R for an Analysis of Variance
R for
15.4: Using Excel and R for an Analysis of Variance
radiation
11.8: Spectroscopy Based on Scattering
radiationless deactivation
11.6: Photoluminescence Spectroscopy
radioactive
14.3: Radiochemistry
Radioactive Analytes
14.3: Radiochemistry
radioactive atoms
14.3: Radiochemistry
radioactive particles
14.3: Radiochemistry
radioactive tracer
14.3: Radiochemistry
radiochemical methods
14.4: Flow Injection Analysis
Radiochemistry
14.3: Radiochemistry
random error
15.3: Validating the Method as a Standard Method
random errors
16.4: Evaluating Quality Assurance Data
random sampling
8.2: Designing a Sampling Plan
range
5.1: Characterizing Measurements and Results
rate
14.2: Chemical Kinetics
rate constant
12.3: Coulometric Methods
14.2: Chemical Kinetics
rate law
14.2: Chemical Kinetics
rate method
14.2: Chemical Kinetics
reactant
7.5: Le Châtelier’s Principle
reactants
7.5: Le Châtelier’s Principle
reaction rate
14.2: Chemical Kinetics
reagent blank
15.2: Verifying the Method
16.3: Quality Assessment
reagent grade
6.1: Analytical Standards
recovery
12.2: Potentiometric Methods
sample
5.4: The Distribution of Measurements and Results
13.4: Gas Chromatography
13.7: Electrophoresis
Sample Cells
10.4: Redox Titrations
R
salt bridge
11.3: UV/Vis and IR Spectroscopy
Sample Collection
8.3: Implementing the Sampling Plan
Redox Titrimetry
Sample Distributions
10.4: Redox Titrations
5.4: The Distribution of Measurements and Results
reducing agent
Sample Introduction
7.4: Equilibrium Constants for Chemical Reactions
reduction
11.4: Atomic Absorption Spectroscopy
Sample Means
7.4: Equilibrium Constants for Chemical Reactions
reference electrode
5.6: Statistical Methods for Normal Distributions
sample preparation
12.1: Overview of Electrochemistry
Reference Electrodes
12.2: Potentiometric Methods
Regression
8.3: Implementing the Sampling Plan
Sample Preservation
8.3: Implementing the Sampling Plan
Samples
6.6: Using Excel and R for a Regression Analysis
Regression Analysis
6.6: Using Excel and R for a Regression Analysis
Regression Equation
6.4: Linear Regression and Calibration Curves
relative supersaturation
9.2: Precipitation Gravimetry
relaxation
11.5: Emission Spectroscopy
Repeatability
5.4: The Distribution of Measurements and Results
13.5: High-Performance Liquid Chromatography
Sampling
4.5: Developing the Procedure
8.1: The Importance of Sampling
8.2: Designing a Sampling Plan
8.3: Implementing the Sampling Plan
Sampling Plan
8.2: Designing a Sampling Plan
8.3: Implementing the Sampling Plan
saturated calomel electrode
5.2: Characterizing Experimental Errors
Reproducibility
12.2: Potentiometric Methods
Scale of Operation
5.2: Characterizing Experimental Errors
Residual Current
12.4: Voltammetric Methods
resolution
11.1: Overview of Spectroscopy
13.2: General Theory of Column Chromatography
13.3: Optimizing Chromatographic Separations
4.4: Selecting an Analytical Method
11.4: Atomic Absorption Spectroscopy
11.6: Photoluminescence Spectroscopy
11.7: Atomic Emission Spectroscopy
scattering
11.8: Spectroscopy Based on Scattering
scientific notation
3.1: Measurements in Analytical Chemistry
response
15.1: Optimizing the Experimental Procedure
scintillation counter
14.3: Radiochemistry
response surface
15.1: Optimizing the Experimental Procedure
SCOT
13.4: Gas Chromatography
retentate
8.6: Classifying Separation Techniques
searching algorithm
15.1: Optimizing the Experimental Procedure
retention factor
13.2: General Theory of Column Chromatography
13.3: Optimizing Chromatographic Separations
retention factors
secondary standards
6.1: Analytical Standards
Selectivity
13.7: Electrophoresis
Retention time
13.2: General Theory of Column Chromatography
robust
4.4: Selecting an Analytical Method
room temperature
7.4: Equilibrium Constants for Chemical Reactions
rugged
4.4: Selecting an Analytical Method
ruggedness testing
4.4: Selecting an Analytical Method
10.2: Acid–Base Titrations
13.3: Optimizing Chromatographic Separations
13.5: High-Performance Liquid Chromatography
13.7: Electrophoresis
14.2: Chemical Kinetics
selectivity coefficient
4.4: Selecting an Analytical Method
8.4: Separating the Analyte from Interferents
selectivity factor
13.2: General Theory of Column Chromatography
15.2: Verifying the Method
8.5: General Theory of Separation Efficiency
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sensitivity
4.4: Selecting an Analytical Method
6.3: Determining the Sensitivity
9.2: Precipitation Gravimetry
10.2: Acid–Base Titrations
Separate Mixtures
13.1: Overview of Analytical Separations
Separation
8.5: General Theory of Separation Efficiency
8.6: Classifying Separation Techniques
8.8: Separation Versus Preconcentration
separation factor
8.5: General Theory of Separation Efficiency
Separation Modules
14.4: Flow Injection Analysis
SFC
13.6: Other Forms of Liquid Chromatography
SHE
12.2: Potentiometric Methods
SI units
3.1: Measurements in Analytical Chemistry
signal
4.3: Classifying Analytical Techniques
6.2: Calibrating the Signal
10.1: Overview of Titrimetry
11.1: Overview of Spectroscopy
13.5: High-Performance Liquid Chromatography
14.4: Flow Injection Analysis
signal averaging
11.3: UV/Vis and IR Spectroscopy
signal processor
11.1: Overview of Spectroscopy
significance test
5.5: Statistical Analysis of Data
Significance Testing
5.5: Statistical Analysis of Data
Significance Tests
5.8: Using Excel and R to Analyze Data
significant figures
3.1: Measurements in Analytical Chemistry
silica
13.5: High-Performance Liquid Chromatography
silica particles
13.5: High-Performance Liquid Chromatography
silver/silver chloride electrode
12.2: Potentiometric Methods
simplex
15.1: Optimizing the Experimental Procedure
Simplex Optimization
15.1: Optimizing the Experimental Procedure
Single Components
12.4: Voltammetric Methods
Single Operator Characteristics
15.2: Verifying the Method
singlet excited state
11.6: Photoluminescence Spectroscopy
slope
6.4: Linear Regression and Calibration Curves
SMDE
12.4: Voltammetric Methods
solid
8.3: Implementing the Sampling Plan
Solids
8.3: Implementing the Sampling Plan
solubility
standard deviation about the regression
7.7: Solving Equilibrium Problems
7.10: Using Excel and R to Solve Equilibrium
Problems
9.2: Precipitation Gravimetry
Standard Error of the Mean
solubility product
7.4: Equilibrium Constants for Chemical Reactions
solute
13.1: Overview of Analytical Separations
solute’s charge
13.7: Electrophoresis
6.4: Linear Regression and Calibration Curves
5.4: The Distribution of Measurements and Results
standard hydrogen electrode
12.2: Potentiometric Methods
Standard Method
15.1: Optimizing the Experimental Procedure
15.2: Verifying the Method
15.3: Validating the Method as a Standard Method
standard operations procedure
solute’s radius
16.2: Quality Control
13.7: Electrophoresis
standard potential
solutions
7.4: Equilibrium Constants for Chemical Reactions
3.5: Preparing Solutions
8.3: Implementing the Sampling Plan
SOP
Standard Reference Materials
5.2: Characterizing Experimental Errors
standard sample
16.2: Quality Control
15.2: Verifying the Method
Soxhlet extractor
8.6: Classifying Separation Techniques
Specificity
4.4: Selecting an Analytical Method
Spectral Interferences
11.7: Atomic Emission Spectroscopy
spectral searching
11.3: UV/Vis and IR Spectroscopy
spectrofluorimeter
standard state
7.2: Thermodynamics and Equilibrium Chemistry
standardization
6.3: Determining the Sensitivity
Standardizing
10.2: Acid–Base Titrations
10.4: Redox Titrations
Standards
12.2: Potentiometric Methods
11.6: Photoluminescence Spectroscopy
13.5: High-Performance Liquid Chromatography
Spectrophotometer
11.3: UV/Vis and IR Spectroscopy
spectrophotometric titration curve
10.3: Complexation Titrations
spectrophotometry
15.1: Optimizing the Experimental Procedure
Spectroscopic Detectors
13.5: High-Performance Liquid Chromatography
Spectroscopic methods
11.5: Emission Spectroscopy
spectroscopy
static mercury drop electrode
12.4: Voltammetric Methods
stationary phase
13.1: Overview of Analytical Separations
13.6: Other Forms of Liquid Chromatography
Stationary Phases
13.1: Overview of Analytical Separations
13.5: High-Performance Liquid Chromatography
statistical analysis
5.5: Statistical Analysis of Data
statistical control
16.1: The Analytical Perspective—Revisited
statistical methods
4.3: Classifying Analytical Techniques
11.1: Overview of Spectroscopy
11.2: Spectroscopy Based on Absorption
11.8: Spectroscopy Based on Scattering
14.4: Flow Injection Analysis
spike recovery
16.3: Quality Assessment
16.4: Evaluating Quality Assurance Data
splitless injection
5.6: Statistical Methods for Normal Distributions
15.3: Validating the Method as a Standard Method
stock solution
3.5: Preparing Solutions
stoichiometric
3.3: Stoichiometric Calculations
stoichiometric relationship
3.3: Stoichiometric Calculations
13.4: Gas Chromatography
SPME
13.4: Gas Chromatography
Spreadsheets
3.6: Spreadsheets and Computational Software
stacking
stoichiometry
4.4: Selecting an Analytical Method
11.3: UV/Vis and IR Spectroscopy
stratified sampling
8.2: Designing a Sampling Plan
Stray radiation
11.2: Spectroscopy Based on Absorption
13.7: Electrophoresis
stripping voltammetry
standard
6.5: Blank Corrections
12.2: Potentiometric Methods
15.1: Optimizing the Experimental Procedure
Standard Additions
6.3: Determining the Sensitivity
12.2: Potentiometric Methods
standard deviation
12.4: Voltammetric Methods
strong acid
7.4: Equilibrium Constants for Chemical Reactions
7.8: Buffer Solutions
strong acids
10.2: Acid–Base Titrations
strong base
5.1: Characterizing Measurements and Results
15.3: Validating the Method as a Standard Method
16.4: Evaluating Quality Assurance Data
10
7.4: Equilibrium Constants for Chemical Reactions
7.8: Buffer Solutions
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strong bases
TISAB
10.2: Acid–Base Titrations
sublimation
8.6: Classifying Separation Techniques
8.3: Implementing the Sampling Plan
10.1: Overview of Titrimetry
10.4: Redox Titrations
10.5: Precipitation Titrations
titrant
10.1: Overview of Titrimetry
10.5: Precipitation Titrations
14.2: Chemical Kinetics
supercritical fluid
8.6: Classifying Separation Techniques
supercritical fluid chromatography
13.6: Other Forms of Liquid Chromatography
Titration
10.2: Acid–Base Titrations
titration curve
10.3: Complexation Titrations
10.5: Precipitation Titrations
supernatant
9.2: Precipitation Gravimetry
surface adsorbates
3.2: Concentration
symmetric equivalence point
10.4: Redox Titrations
systematic errors
15.3: Validating the Method as a Standard Method
16.4: Evaluating Quality Assurance Data
10.1: Overview of Titrimetry
10.4: Redox Titrations
10.5: Precipitation Titrations
titration error
10.5: Precipitation Titrations
Titrimetry
4.3: Classifying Analytical Techniques
10.1: Overview of Titrimetry
10.2: Acid–Base Titrations
10.3: Complexation Titrations
10.4: Redox Titrations
10.5: Precipitation Titrations
systematic–judgmental sampling
tolerance
5.2: Characterizing Experimental Errors
target population
8.1: The Importance of Sampling
TCD
13.4: Gas Chromatography
technique
4.2: Techniques, Methods, Procedures, and Protocols
temperature
7.2: Thermodynamics and Equilibrium Chemistry
13.4: Gas Chromatography
Temperature Control
13.4: Gas Chromatography
Temperature programming
13.4: Gas Chromatography
Tempmperature
10.2: Acid–Base Titrations
total analysis technique
4.3: Classifying Analytical Techniques
total charge
12.3: Coulometric Methods
total ionic strength adjustment buffer
12.2: Potentiometric Methods
Total Mobility
theory
9.2: Precipitation Gravimetry
Thermal Conductivity Detector
13.4: Gas Chromatography
thermal excitation
11.5: Emission Spectroscopy
thermodynamically
7.2: Thermodynamics and Equilibrium Chemistry
thermodynamics
13.7: Electrophoresis
9.3: Volatilization Gravimetry
thermogravimetry
9.3: Volatilization Gravimetry
unpaired data
5.6: Statistical Methods for Normal Distributions
unweighted linear regression
V
validation
4.5: Developing the Procedure
15.3: Validating the Method as a Standard Method
van Deemter equation
13.3: Optimizing Chromatographic Separations
vanadium
15.1: Optimizing the Experimental Procedure
Variance
5.1: Characterizing Measurements and Results
8.2: Designing a Sampling Plan
15.3: Validating the Method as a Standard Method
15.4: Using Excel and R for an Analysis of Variance
Variations
13.3: Optimizing Chromatographic Separations
vibrational energy level
11.6: Photoluminescence Spectroscopy
11.6: Photoluminescence Spectroscopy
Visualizing Data
6.5: Blank Corrections
5.8: Using Excel and R to Analyze Data
tracer
Vmax
14.3: Radiochemistry
14.2: Chemical Kinetics
transducer
11.1: Overview of Spectroscopy
transmittance
11.2: Spectroscopy Based on Absorption
11.3: UV/Vis and IR Spectroscopy
trip blank
16.3: Quality Assessment
triplet excited state
11.6: Photoluminescence Spectroscopy
turbidimetry
11.8: Spectroscopy Based on Scattering
type 1 error
5.5: Statistical Analysis of Data
type 2 error
5.5: Statistical Analysis of Data
7.2: Thermodynamics and Equilibrium Chemistry
thermogram
3.2: Concentration
units
vibrational relaxation
total Youden blank
theoretical model
15.1: Optimizing the Experimental Procedure
3.2: Concentration
unit conversion
6.4: Linear Regression and Calibration Curves
titrations
8.2: Designing a Sampling Plan
T
14.2: Chemical Kinetics
unit
10.1: Overview of Titrimetry
Systematic Sampling
8.2: Designing a Sampling Plan
Uncompetitive Inhibition
3.2: Concentration
Titration Curves
9.2: Precipitation Gravimetry
symbolic notation
3.1: Measurements in Analytical Chemistry
5.2: Characterizing Experimental Errors
5.3: Propagation of Uncertainty
6.4: Linear Regression and Calibration Curves
11.3: UV/Vis and IR Spectroscopy
15.1: Optimizing the Experimental Procedure
titrand
subsamples
substrate
uncertainty
12.2: Potentiometric Methods
void time
13.2: General Theory of Column Chromatography
Volatilization
9.3: Volatilization Gravimetry
volatilization gravimetric
9.4: Particulate Gravimetry
Volatilization Gravimetry
9.1: Overview of Gravimetric Methods
9.3: Volatilization Gravimetry
Volhard method
10.5: Precipitation Titrations
Voltammetric Measurements
12.4: Voltammetric Methods
voltammetric methods
12.4: Voltammetric Methods
U
Voltammetric Technique
ultramicro
voltammetry
12.4: Voltammetric Methods
4.4: Selecting an Analytical Method
thermometric titration curve
12.4: Voltammetric Methods
13.5: High-Performance Liquid Chromatography
voltammogram
10.1: Overview of Titrimetry
Time
12.4: Voltammetric Methods
4.4: Selecting an Analytical Method
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Voltammograms
12.4: Voltammetric Methods
volume
3.4: Basic Equipment
4.3: Classifying Analytical Techniques
volume percent
3.2: Concentration
volumetric buret
10.1: Overview of Titrimetry
volumetric flask
3.4: Basic Equipment
volumetric pipet
3.4: Basic Equipment
W
Weight percent
3.2: Concentration
wavelength
11.1: Overview of Spectroscopy
11.7: Atomic Emission Spectroscopy
11.8: Spectroscopy Based on Scattering
wavenumber
where
15.1: Optimizing the Experimental Procedure
working electrode
12.1: Overview of Electrochemistry
12.3: Coulometric Methods
13.5: High-Performance Liquid Chromatography
11.1: Overview of Spectroscopy
weak acid
7.7: Solving Equilibrium Problems
10.3: Complexation Titrations
weak acids
Z
Zeta Potential
7.4: Equilibrium Constants for Chemical Reactions
weak base
13.7: Electrophoresis
7.8: Buffer Solutions
12
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